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TRANSACTIONS

OF THE

AMERICAN INSTITUTE

OF

CHEMICAL ENGINEERS

VOLUME V
1912

Office of the Secretary

POLYTECHNIC INSTITUTE

Brooklyn, N. Y.

PUBLISHED BY THE INSTITUTE
AND FOR SALE BY

D. VAN NOSTRAND COMPANY

NEW YORK
1913

7P

I

The Institute as a body does not hold itself responsible for the
statement of facts or opinions advanced in papers or discussions.

Copyright, 1913, by

AMERICAN INSTITUTE OF

CHEMICAL ENGINEERS

CONTENTS

ADDRESSES AND PAPERS READ BEFORE THE INSTITUTE

PAGE

Phenol-Formaldehyde Condensation Products. L. H. Baekeland, i

Protection of Intellectual Property in Relation

to Chemical Industry L. H. Baekeland, 19

Notes on a Study of the Temperature Gradients

of Setting Portland Cement Allerton S. Cushman, 43

The Production of Available Potash from the / Allerton W. Cushman and

Natural Silicates \ George W. Coggeshall, 52

Potash, Silica and Alumina from Feldspar. . . .Edward Hart, 68

A Chemical Investigation of Asiatic Rice. . . .Allerton S. Cushman and

H. C. Fuller, 70

The Beehive Coke Oven Industry of the

United States A. W. Belden, 78

Action of Disinfectants on Sugar Solutions . . . George P. Meade, 88

The Decomposition of Linseed Oil During / J. C. Olsen and

Drying I A. E. Ratner, 100

Tests on the Opacity and Hiding Power of

Pigments G. W. Thompson, ioS

Control of Initial Setting Time of Portland

Cement E. E. Ware, rig

The Effect of "Lime-Sulphur" Spray Manu-
facture on the Eyesight James R. Withkow, 127

Acetylene Solvents . J. H. James, 133

The New Chemical Engineering Course and

Laboratories at Columbia University M. C. Whitaker, 150

The Need of Standard Specifications in Oils for

Paving Block Impregnation John Hayes Campbell, 170

The Presence of Oxygen in Petroleums and

Asphalts Sam. P. Sadtler, 178

The Chemical Engineer and Industrial EtS-

ciency Wm. M. Booth, 184

Water for Industrial Purposes Wm. M. Booth, 197

The Availability of Blast Furnace Slag as a

Material for Building Brick Albert E. White, 204

IV CONTENTS

PvCB

Technical Accounting and CJicmical Control in

Sugar Manufacture David L. Davoll, Jr., 220

The Hituminous RocivS of the United States

and Their Use for Street Surfaces S. F. Peckham, 245

Code of Ethics 255

Constitution 259

Officers and Committees for 1913 266

Membership List 269

Index 281

TRANSACTIONS OF THE AMERICAN INSTI-
TUTE OF CHEMICAL ENGINEERS

PHENOL-FORMALDEHYDE CONDENSATION
PRODUCTS

By L. H. BAEKELAN'D, ScD., Yonkers, N. T.

Read at Joint Meeting with the Eighth International Congress, New York
City, September 4-13, 1912.

The resinous or amorphous products resulting from the action
of phenolic bodies upon formaldehyde have lately attracted con-
siderable attention on account of their rapidly increasing applica-
tions for industrial purposes.^

It is questionable whether this general designation of "condensa-
tion products of phenols and formaldehyde'' should be maintained
much longer. Indeed, it is well known that these products can be
obtained without the use of so-called formaldehyde. In fact, the
first condensation products thus described were produced without
the use of formaldehyde,- and it is generally accepted that other
methylene compounds, for instance, methylal, trioxymethylen, hexa-
methylentetramin, etc., can replace formaldehyde in this reaction.
The fact that hexamethylentetramin can suitably replace formalde-
hyde in the formation of the infusible phenolic condensation

1 Baekeland : "The Synthesis. Constitution and Uses of Bakelite," Journal
of Industrial and Engineering Chemistry, Vol. i. No. 3, 1909, page 149. "On
Soluble, Fusible, Resinous Condensation Products of Phenols and Formalde-
hyde," Journal of Industrial and Engineering Chemistry. Vol. i, Xo. 8, 1909,
page 545. "Recent Developments in Bakelite," Journal of Industrial and
Engineering Chemistry," Vol. 3, No. 12, igil, page 932.

= Berichte, 5, p. 1905; 19, pp. 3004 and 2009; 25, p. 241 1.

2 AMERICAN INSTITUTE OP CHEMICAL ENGINEERS

products was published as far back as December 31, 1907, by
Lebacli/

Lately, I have succeeded in producing fusible resinous conden-
sation products identical with those described by Blumer, DeLaire,
etc* by introducing a mixture of salicylic acid and an inorganic
acid in the cathode compartment of an electrolytic cell in which
sodium chloride is electrolyzed, a mercury catliode being used.
According to the well know reaction of Kolbe. the carboxyl group
of salicylic acid is introduced by reacting with CO. on phenolate
of sodium. So that we have here an example of the possibility of
introducing indirectly the methylene group as CO-,, then reducing
the carboxyl group by means of nascent hydrogen. A similar obser-
vation has already been recorded by \'elden,° who expected to get
oxybenzyl-alcohol by reducing salicylic acid but obtained the cor-
responding saliretin-body resulting from the dehydration of phenol
alcohol.

However, the designation "phenol-formaldehyde condensatiort
products" has been so generally used, that for awhile at least, we
shall have to submit to it as a matter of routine.

In the same way, we are erroneously designating as "formalde-
hyde" a commercial aqueous solution containing some real formalde-
hyde or methylen-oxide, CHjO, with much methylenglycol, methylal,
trioxymethylene. hydrates of trioxvmethylene, other polyoxymethy-
lens, etc., all compounds of mcthylen of which the technical value is
equivalent in this reaction to that of true formaldehyde."

The direct relationship of the resinous condensation products to
phenol-alcohols or their anhydrides, seems now pretty well estab-
lished. The so-called fusible soluble resinous condensation products
are merely varieties of the saliretins," and all these products differ

3 Knoll patent, Belgium, No. 204,811. December 31, igo/. Ditto. Wetter
(Knoll) British patent No. 28009, 'PO/. owned by the Bakelite Gesellschaft of
Berlin.

* Baekeland, "On Soluble, Fusible, Resinous Condensation Products of
Phenols and Formaldehyde."

* Velden. Journ. Prak Chemie.. (2) 15, p. 164. Jahresbericht. 1877, p. 337.

* Raikov. Chem. Ztg., 26, 135; 12, 11 (1901). Kekule, Ber.. 23. 2435.
Harries, Ber., 34, 635. Compt. rend., 124, 1454: Bull. soc. chim. 17, 840.
F. .\uerbach. also Auerbach and Barschall, Arb. kais. Gesundh.. Band XXII,
Heft 3 and Band XXVII, Heft i. Verlag Julius Springer. Berlin.

' Beilstein, Organ. Chemie, Vol. 2, 1896, p. 1109. R. Piria, Ann. Chem.,

PHENOL-FORMALDEHYDE COM DENS ATION PRODUCTS 3

from each other only by greater or lesser fusibility, solubility, or
hardness, and each of these properties can be modified at will.
Furthermore, we have the means at hand of producing all these
bodies directly from phenol-alcohols.*

The formation of ortho- and para-oxybenzyl-alcohol, or their
homologs, by Manasse and Lederer, is sufficiently well known.^
This process consists in the direct action of one molecule of phenol
on one molecule of formaldehyde in presence of one molecule of
NaOH under special conditions.

Then DeLaire^" showed that these same phenol-alcohols can be
transformed industrially, by dehydration, into fusible resins or sal-
iretin products suitable for commercial purposes in place of shellac,
copal, or other natural resins. In that process, it is not necessary
to first produce the phenol-alcohol in pure form, and the two
reactions can be carried out practically at the same time, so that
the phenol-alcohol is dehydrated to saliretin resins as soon as it
forms.

This is accomplished more directly by reacting with phenol on
formaldehyde in presence of an acid,^' provided the reaction be
carried out under suitable conditions. One of the required con-
ditions is that the phenol should be in excess so as to avoid the
formation of variable amounts of infusible and insoluble products.
A fusible soluble saliretin can thus easily be prepared which has all
the appearance of a resin ; it melts if heated and solidifies by cool-
ing ; it is soluble in alcohol and acetone ; it can be maintained in
fusible condition for very long periods, without becoming infusible
or insoluble, provided heating be carried on below certain tempera-

48. 75; 56, 37; 81, 245: 96, 357. Moitessier, Jahresbericht, 1886, p. 676.
K. Kraut, Ann. Chem., 156, 123; Gerhardt, Ann. Chim. Phys. (3) 7, p. 215.
F. Beilstein and F. Seelheim, Ann Chem. 117, p. 83. C. Schotten, Berichte,
1878, p. 784.

* Baekeland, "On Soluble, Fusible, Resinous Condensation Products of
Phenols and Formaldehyde," Journal Industrial and Engineering Chemistry,
Vol. I, No. 8, 1909, p. 545.

'Journal Praktische Chemie (2), vol. 50, p. 224. Ber., 1894. 2409-241 1;
D. R. P., Bayer, 85588 ; U S. P., Manasse, 526,786, 1894.

I" DeLaire, British Patent, 15517. 1905; D. R. P., 189,262.

'' Blumer, Brit. Pat., 6823, 1903 ; 12880, 1902 : DeLaire, French Patent,
361,539; Wetter (Knoll), Brit. Pat., 28009, 1O07; Knoll, French Pat., 39S>6S7;
Bayer, D. R. P., 237,786; D. R. P., 201,261 ; Brit. Pat., 26317, 1907, etc.

4 AMERICAN INSTITUTE OF CUEMICAL ENGINEERS

turcs, and provided the excess of phenol be not removed. This
fusible resin and its preparation has been described by lilumer, and
DeLaire as a "shellac substitute," or "resin substitute" ;'* by Baeke-
land, who calls it "Novolak,""" and lately again by Aylsworth, who
calls it "phenol resin."'* In whatever way it be obtained, whether
by using a phenol-alcohol (DeLaire, Baekeland) ; whether by start-
ing from phenol and formaldehyde in the presence of oxyacids
{ Blumer), or in the presence of mineral acids (DeLaire, Thurlow,
Bayer), or by the action of phenol on formaldehyde without adding
condensing agents, ( Story )"* (or Aylsworth)'* the product is
absolutely the same in its chemical and physical properties. Its
melting point or fusibility may be modified at will by varying the
amount of free phenolic body. This free phenol exists in solid
solution in the mass and can be eliminated by merely physical
methods ; by the partial elimination of this free phenol, the fusibility
and the solubility of the rosin arc decreased. The last traces of free
phenol cling tenaciously to these salirctin resins ; so much, indeed,
that at one time, I was inclined to believe that this small amount of
phenol was chemically combined. Indeed, the last traces of phenol
cannot be exjjelled by heating at the lower melting temperatures of
the product. There is nothing strange in this, if we take into con-
sideration that phenol itself has a relatively high boiling point, and
we know of numerous examples where colloids retain, physically,
small amounts of other bodies which form therewith colloidal solid
solutions. As long as there is some excess of phenol present in the
saliretin, it is possible to maintain the mass in fusion for a practi-
cally indefinite time, provided the temperature be not raised too
high. Pure saliretin, containing no excess of phenol, may be kept
in fusion for some time, but after awhile it polymerizes and becomes
less fusible until finally it changes into some infusible product.
However, it should be noted right here that this latter product,
although it is infusible, does not possess the maximum mechanical
strength nor hardness, nor general chemical and physical resistivity,
of those other polymerized infusible products, of which I will speak

'=Loc. cit.

"Journal Industrial and Engineering Chcmistr>', 1909, p. 545.

"U. S. Pat. 1,029,737.

"Austrian Pat. 30844. p. 2, 1. 17 to 20.

" Loc. cit.

PIIENOI^FORMALDEHYDE CONDENSATION PRODUCTS 5

later on, and which are obtained by reacting with a sufficiently larger
amount of formaldehyde, or equivalent methylen compounds, and
which have been designated as Bakelite C.

It is possible to expel the slight excess of phenol which lends
special fusibility to the so-called fusible resins ; this can be accom-
plished whether these resins be called "shellac substitutes,"
"•Kovolak," or "phenol resins," or whether they be made directly
from phenol alcohols, or from phenol and formaldehyde with or
without acid condensing agents. Indeed, plain heating at 300° C. to
350° C. or better, heating in vacuo, or in a current of an inert gas,
like nitrogen, easily expels the free phenol, and produces infusibility.
The same result is readily obtained by entraining the free phenol, by
blowing superheated steam through the molten resinous mass.

These facts are corroborating proofs to others which establish
clearly the saliretin nature of these fusible products, and demon-
strate their relationship to the phenol-alcohols from which they are
derived. If these fusible resins are prepared directly from phenol
and formaldehyde, the preliminary formation of phenol-alcohol may
escape our notice, because by the action of heat on the mixture,
especially in presence of acid bodies, the phenol-alcohols are rapidly
dehydrated to saliretin products. But it is quite possible to demon-
strate their presence, and my assistant, Dr. A. H. Gotthelf, while
preparing fusible resinous condensation products, by boiling a
mixture of phenol and formaldehyde, acidulated by means of HCl,
has been able to extract from this mixture well defined crystals of
oxybenzyl-alcohol before the heat had accomplished its resinifying
action.

It is self-evident that as soon as high temperatures are applied to
such mixtures, the formed phenol-alcohol will quickly undergo
resinification, because the phenol-alcohol will be dehydrated to a
saliretin product as soon as it is formed.

If there is an excess of phenol present, or if the formaldehyde
reacts in insufficient proportions, which amounts to the same thing,
a fusible saliretin will be the result.

In the absence of an excess of phenol, but using however, a
restricted amount of formaldehyde or other methylen compound, a
polymerized infusible saliretin will be produced.

But whenever we succeed in bringing into reaction a sufficient
amount of formaldehyde or its equivalent, then a much harder.

6 AMERICAS INSTITUTE OF CHEMICAL ENGINEERS

much stronger and more resistive infusible body than an infusible
saliretin will be formed, and this body of maximum strength and
resistivity is identical with Bakelite C.

If we first produce the pure crystalline phenol-alcohol, contain-
ing no excess of phenol, for instance crystalline saligenin or
oxybenzyl-alcohol, and if we heat it gently, it will simply dehydrate
and be transformed in a fusible mass which on cooling, solidifies to
a resinous product — a fusible saliretin resin. The latter, submitted
to the further action of heat, polymerizes and becomes an infusible,
insoluble saliretin. This polymerization is facilitated, by the pres-
ence of small amounts of catalyzers, for instance, hydrochloric acid.
The presence of an excess of phenol retards iiolymerization ; hence
the infusibility induced by polymerization will be retarded, and
this, until some way or another the excess of phenol has been
expelled. The infusible polymerized saliretin obtained by heating
phenol-alcohols containing no free phenol, or by heating fusible
saliretin containing no free phenol, is insoluble in alcohol, but swells
in acetone; it softens decidedly on heating, although it is no longer
fusible. Longer heating does not harden it further, nor make it
more resistive. It is harder, stronger, and more resistant to physical
and chemical agents than the fusible saliretin from which it is
derived ; in this respect, it surpasses even more the soluble fusible
resins described by Blumer," DeLaire," Baekeland," and called
"phenol resin by Aylesworth.'' But even after polymerization or
hardening has been carried as far as possible, it is considerably less
hard and less strong and less resistant to physical and chemical
agents than the polymerization products resulting from the reaction
of phenol on a sufficiently large proportion of formaldehyde or
equivalent substances.

In order to obtain the latter polymerization products of maxi-
mum strength, hardness, and maximum resistivit)', an ade(|uately
larger amount of methylen group must be introduced before or dur-
ing the act of polymerization. The introduction of this methylen
group may be accomplished by at least three distinct metiiods:

First method: Reacting directly with a sufficient amount ot
formaldehyde, or its equivalents upon phenol.

Second method : Reacting with formaldehyde or its equivalent
on phenol-alcohol.
'* Loc. cit.

PHENOL-FORMALDEHYDE CONDENSATION PRODUCTS

PHENOL+ FORMALDEHYDE (OR EQUIVALENTS) UNDER VARYING
REACTING CONDITIONS FORM DIFFERENT BODIES.

GROUP I

Inilia! or parlia! condensation produclor
Product A, liquid, pasty, or solid, but
fusible and soluble.

Product B or in-
termediate prod-
uct: (Brittle when
cold, elastic when
hot, but infusible;
swells in acetone
without dissolving.
By further applica-
tion of heat is
transformed in final
Product C.)

GROUP II

Phenol-alcohols: oxyben-
zylalcohol saligenin, etc.

Y

Products of dehydration: Fusi-
ble and soluble, with or without
e.xcess of phenol; called by differ-
ent authors: Saliretin, or salirclin
resins: '' Shellac' or Resin stibsti-
stitules" (Blumer, DeLaire, etc.);
"Novolak" (Baekeland); "Phen«
ol-resin" (Aylsworth).

Final Product C, infusible, insoluble,
and of maximum hardness, strength and
resist! V ty. Called by different authors:
"Bakelite C," "Final condensation prod-
uct,' "Ultimate infusible product,"
"Inusible phenolic-condensation prod-
uct." Hardness, strength, and resistiv-
ity decidedly superior to that of the end
product of Group II.

Y

Polymerized saliretins: sub-
stances of limited solubility or
insoluble and of high melting-
point or infusible. Less hard,
less strong, and less resistive than
Bakelite C.

8 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

Third method: Producing a fusible dehydration product of
phenol-alcohols or saliretin products, then reacting thereon with
formaldehyde or its equivalents.

The following diagram describes very well all these relations:

First or Direct Method. Direct Action of Phenol
on i-'ormaldeiiyde.

Phenol can be made to react on formaldehyde or its equivalents
at sufficiently high temperature to produce directly an infusible
insoluble polymerization product of maximum strength and hard-
ness ( Bakelite C). In this reaction, the main requirement is that a
sufficient amount of formaldehyde or its e(|uivalents should enter
into reaction. For this purpose, it is not necessary nor sufficient
that the required amount of formaldehyde be merely present, because
some of the formaldehyde may not enter into reaction or be lost
during the operation. The principal requirement is that the formal-
dehyde should react in sufficient amount on at least a portion of the
])henol present, even if some of the latter remains uncombined in the
mass.

By the use of suitable methods, this reaction can be interrupted
at its initial stages, so as to produce initial or partial condensation
l)roducts, which are temporarily fusible and soluble before further
application of heat has changed them. These initial condensation
products may be liquid, or pasty, or under specially favorable con-
ditions, for instance, by the use of small amounts of some bases, they
may be prepared in solid form. At any rate, they are soluble in
alcoliol and acetone, and the solid variety is fusible. These fusible
soluble initial products should not be confounded with the further
advanced and intermediate jiroduct B, as described in my paper on
"The Synthesis, Constitution and Uses of Bakelite,"'* because the
latter is insoluble and infusible, although it has not ac(]uired the
maximum hardness and resistivity which further application of heat
will bring forth by changing it to condition C.

Further action of heat upon these fusible and soluble initial
condensation products will ultimately cause polymerization and pro-
duce the final infusible and insoluble product of maximum hard-
's Journal Industrial and Engineering Chemistry, Vol. I, No. 3. 1909,
p. 149-

PHENOL-FORMALDEHYDE CONDENSATION PRODUCTS 9

ness, maximum strength, and maximum chemical resistivity.
(Bakelite C).

By heating mixtures of phenol and formaldehyde in suitable
proportions, at sufficiently high temperatures, for a sufficiently long
time, chemical condensation may take place without the addition
of condensing agents or catalytic agents ; however, under such
unfavorable conditions, the action is too slow and too difficult to
control, for technical purposes.

By the addition of acids or acid salts, the reaction may be
hastened to the point of becoming violent. But the presence of
acid bodies tends to develop disturbing side-produce which lessen
the technical value of the final product. Furthermore, in presence
of the acid-reacting mixture, whenever there is sufficient excess of
phenol, we do not obtain the infusible, final product, but resins
of the fusible saliretin or "shellac substitute" type. Things go
quite differently if small amounts of bases are present during the
reaction.'" Small quantities of bases prevent radically the forma-
tion of fusible soluble saliretin products (shellac substitutes, Novo-
lak. phenol-resin, etc.) and insure the formation of infusible, insolu-
ble, final products, even in presence of a decided excess of phenol.
If the phenol be used in excess, it will be found in the final product
as a solid solution. In fact, the excess of phenol may be exag-
gerated to the point that the final product becomes very flexible or
assumes a gelatinous appearance, and swells considerably in certain
solvents, like phenol, or alcohol, or acetone, without, however, enter-
ing into complete solution. In any case this free-phenol-containing
substance is infusible; in other terms, the application of heat can
no longer liquefy it, although higher temperatures may char or
destroy it.

This behavior of the bases constitutes a radical dift'erence with
that of acids or other acid-reacting bodies. Whenever acid-reacting
bodies are used in conjunction with an excess of phenol, or an insuf-
ficient amount of reacting formaldehyde ( which amounts to the same
thing), they tend to produce fusible, soluble resins, while under
exactly the same conditions and with the same proportions of phenol
and formaldehyde, small amounts of bases develop surely infusible
polymerized bodies as ultimate products.

In this method, the bases should be used in relatively moderate

i!>See Baekelaiid, U. S. P., 942,809.

10 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

amounts ; not in molecular proportions, as Manasse and Lederer^"
utilize them for making ])hcnol-alcohols, nor as DeLaire-" employs,
them to produce the fusible resinous dehydration products of these
phenol-alcohols. Neither should they be used in such large quanti-
ties nor under such conditions as Hentschke-' recommended for the
manufacture of certain antiseptic compounds.

If the amount of base be jiroperly restricted, the reaction pro-
ceeds very regularly and remains under easy control. The base
acts as an excellent accelerator, both in the condensation and in the
polymerization. The use of bases under above mentioned condi-
tions enables one to carry out the reaction \vit)i utmost uniformity
and certainty of results.

At first sicjitt, the iiiifortancc of these seemingly modest facts is
not very a(<['arciit: no more than the value of the observation that
sufficient countcrj^ressure permits quick polymerization ai high
temperatures li'ithout risk of porosity; no more indeed than the
realization of the fact that the final product with its great hardness,
its strength and other splendid qualities, is unelastic and ivoc fully
deficient for most industrial purposes zvhere great resistance to
shock or vibration is required, and that the incorporation of suitable
fibrous materials improves all this by modifying the shattering Zi'otr
induced by impact. Yet these are the three main factors ichich have
enabled us to harness into technical service an elusive laboratory
reaction, and have rendered possible the creation of a nezu industry
ivhich is gaining daily in importance.

It has been shown-- that small amounts of ammonia, or amines
may be used to good advantage for this purpose. It is a well-known
fact-' that ammonia or ammonium salts, in presence of formalde-
hyde produces instantly a corresponding amount of hexamethylente-
tramin. In the same way, if any ammonia be added to a mixture of
phenol and formaldehyde, a corresponding amount of hexamethyl-
entetramin is produced which can easily be extracted from the
mixture. This fact was contirmed by Lebach, and can easily be

-" Loc. cit.

"Hentschke. D. R. P., 157,553.

"Baekeland, U. S. Pat., 942,809.

=3 VVohl, Ber., 19, 1892; Tollcns, Her., 17, 653; Carl Goldschmidt, p. 29;
Bonn. Vcrlag von Friedrich Cohn, 1903; Cambier, Brochct, Compt. rend.,
120, p. 557.

PHEXOL-ICRMALDEHFDE CONDENSATION PRODUCTS 11

ascertained by direct experiment.-* It is self-evident that instead
of a mixture of phenol and formaldehyde and ammonia, an equiva-
lent amount of hexamethylentetramin or hexamethylentetramin-
triphenol-" may be used. So that in the preparation of these bodies,
formaldehyde can be replaced by hexamethylentetramin. This was
already published by Lebach in the patent literature as far back
as the end of 1907.-" Whether the phenol mixture be prepared
with ammonia or with hexamethylentetramin, its properties are
practically the same, and on heating both mixtures engender the
same product, with final evolution of ammonia gas.

Whatever be the methods employed, this reaction is strongly
exothermic, and heat is set free in the two phases of the reaction:
first, in the condensation stage, by which the initial product is
formed, and water is separated ; second, in the final hardening
when the product becomes infusible by polymerization, a considera-
ble disengagement of heat takes place anew. If the substance be
heated in thin layers, this self-heating may be unobservable on
account of the heat losses, under such conditions; if, however, the
mass is thicker or bulkier, and more especially if it be contained in
a mold, this self-heating becomes very disturbing, and liberates gas-
eous or volatile products which cannot escape before the mass sets
to infusibility ; this causes the mass to swell and raise and to become
porous, and makes it practically worthless for almost all technical
purposes. This was the stumbling block which former investiga-
tors tried to avoid by conducting the hardening at very low tempera-
tures or by the use of suitable solvents which tend to moderate the
reaction. This tendency towards foaming exists also if acid-condens-
ing agents are used, or even if no catalytic agents are added at all.
The liberated gaseous products may vary according to conditions ; in
some cases they may consist largely of formaldehyde gas, which
tends to escape before the reaction is accomplished ; if ammonia
be used, and more so if hexamethylentetramin be employed, varying
amounts of ammonia gas will be set free.

Specially when hexamethylentetramin is used, the evolution

"* Lebach, Zeitschrift angewandte chemie., 1909, p. 1600.
-5 The addition product of phenol and hexamethylentetramin. See Beil-
stein, Handbuch der Organischen Chemie,' Third Edition, Vol. II, p. 651.

=" Knoll Belgian patent, loc. cit., and Wetter (Knoll), British patent,
loc. cit.

12 AMERICAN INSTITUTE OF CUEMICAL ENGINEERS

of ammonia is very abundant, and this naturally increases the
tendency to foam and to give a porous final [jroduct. This tendency
to foam becomes pronounced only at temperatures above ioo° C,
because at these increasing tem|)cratures the exothermic reaction
sets in. Jt should be noted that temperatures considerably higher
than 1 00° C arc those which are employed in almost all commercial
applications of these products, because they allow quick hardening
and quick molding. At such high temperatures, polymerization pro-
ceeds very rapidly, but the exothermic reaction su])erinduces a
furtlier spontaneous increase of the temperature of the mass, and in
this way tlie defect of foaming is considerably more pronounced.

This tendency to foam makes it of the utmost technical impor-
tance, whenever high temperatures are employed, for quick com-
mercial work, that the liberation of gaseous or volatile products
during the polymerization or hardening process should be opposed
by a suitable counter-pressure. The latter may be applied in various
ways; for instance, by heating in closed molds, or in closed vessels,
so that the imprisoned gases develop a suitable counter-pressure ; or
by heating in a chamber in which air or other gases have first been
pumped to a suitable pressure; or by heating in a hydraulic press.
In the latter case, the first function of the pressure is to counteract
the development of gaseous products, while at the same time, the
mass is given the desired shape in the mold. Baekeland, U. S.
Patent, No. 942,699.

For other applications, like varnishes or lacquer, where the
material is applied in thin layers, the use of counter-pressure is not
indispensable.

As stated above, the use of ammonia or hexamethylcntetramin
increases the tendency to foam. On the other hand, small amounts
of tixed alkalies, like caustic soda, act as more powerful accelators
than ammonia or hexamethylentetramin, without causing the evolu-'
tion of disturbing ammonia gas or other gases. In this, and other
respects, the fixed alkalies have decided advantages over ammonia
or hexamethylentetramin, as well as over acid-condensing agents.
For instance, they permit rapid hardening at the relatively low tem-
peratures of 70° to 95° C. ; furthermore, as soon as the initial solidi-
fication has set in. the temperature can be raised quickly to 1 10°, 120°,
160° C. At these higher temperatures, the hardening proceeds with
great intensity and without fear that the gas bubbles should cause

PHENOL-FOKMALDEHYDE CONDENSATION PRODUCTS 13

porosity. If the heating be carried to the hardening temperature,
before all the water has been first expelled, then the only necessary
precaution will be to keep the temperature sufficiently below ioo° C,
so that no steam should be evolved, which might cause blisters;
but as soon as the mass has been heated long enough at these lower
temperatures, so that it has solidified sufficiently, the temperature
can be raised with impunity above the boiling point of water. As
soon as these higher temperatures become available, the polymeriza-
tion to final hardening advances very rapidly.

For many purposes, it is simpler to drive off the water at tem-
peratures below the polymerization temperature, either by drying in
vacuo, or by drying in a stove at ordinary pressure at moderate tem-
peratures, for instance, 50° C. or below. Such dried material can
now be submitted directly to relatively high temperatures without
risk of blistering or foaming. This gives us the very best means for
rapid hardening, as required by commercial processes. The use of
these fixed alkalies has enabled us to carry on hardening and mold-
ing at a faster rate than is possible with ammonia or hexamethyl-
entetramin, or other means, and at the same time to produce molded
articles of better heat-resisting qualities, of highest resistivity to
solvents, chemicals, and of excellent dielectric properties. For
many electrical purposes, the fact that no free ammonia exists in
the mass, is a further advantage ; indeed, this free ammonia is
slowly liberated by heat from molded articles and sometimes may
play rather disturbing pranks. It has a tendency to corrode brass
articles.

Second Method. Action of Form.'\ldeh\t)e or its Equivalents
ON Phenol Alcohols.

I described this process in 1908.-"

It has been shown that the best results are obtained if the amount
of formaldehyde is at least otie-sixth of a molecule, as calculated
to one molecule of phenol-alcohol. This same ratio holds good if
substances equivalent to formaldehyde or to phenol-alcohols are
used.

-' The Synthesis, Constitution, and Uses of Bakelite, loc. cit. See also
Baekeland, Belgian addition, patent No. 213,576; Baekeland, French addition,
patent No. 11,628.

14 AilERJCAN INSTITUTE OF CUEMICAL ESCIXEERS

This method has enabled us to gain clearer insight in the
relations of all infusible condensation products to the phenol-
alcohols, and has furnished us the theoretical means for detemiining
the optimum quantities of reacting materials in our technical methods
of manufacturing.

However, this process is more of theoretical than of practical
interest, in as far as the third method accomplishes substantially
the same result by starting from the anhydrides of phenol-alcohols.

Third Method. Action of Formaldehyde or Its Equivalents
(Paraform, Hexamethylentetkamin, etc.) on Saliretin-

RESINS.

The method is another indirect method and consists in first pre-
paring a saliretin-resin of tiie fusible soluble type, then reacting
thereupon with formaldehyde or an equivalent of formaldehyde.-'
This method was first published by Lebach at the end of 1907.=°

In these patents, it is clearly mentioned that paraform and
hexamethylentetramin are equivalent to formaldeiiyde in the prepa-
ration of condensation products. Furthermore, it is described how
the condensation products may be prepared in two successive steps
by adding the formaldehyde or hexamethlentetramin, or other
equivalents, in two successive quantities. Briefly stated, the process
consists in first preparing a fusible saliretin-resin, then to this resin
is mixed a second quantity of formaldehyde, paraform, or hexa-
methylentetramin ; this mixture submitted to heat produces the
infusible product "C." In reality, we prepare here, in two steps, a
product which is practically similar to the solid initial condensation
product described in the first or direct method. In that method, the
initial condensation product is obtained more directly by the addi-
tion of a sufficient amount of formaldehyde to phenol, in presence
of ammonia, or other bases, or by the equivalent use of hexamethyl-
entetramin or paraform. In the first or direct method, the reaction
between the phenol and the formaldehyde ensues under elimination
of water due to so-called chemical condensation. In the present

=>» Backcland. U. S. Patent No. 1,038475, granted after interference with
Aylsworth.

=' Knoll, Belgian Patent No. 204.811, Dec. 31. if»7. and Wetter (KnolU,
British patent 28.009, i9or. all owned by the Bakelite Gesellschaft, of Berlin.

PHENOL-FORM ALDEUYDE CONDENSATION PRODUCTS 15

case, however, a portion of the formaldehyde is first made to react
on an excess of phenol, bringing about a corresponding elimination
of water by chemical condensation ; but in as far as the amount
of formaldehyde is insufficient, fusible saliretin-resin is formed. In
order to transform the latter into the product "C," it is necessary to
supply an additional amount of formaldehyde, or some paraform, or
hexamethylentetramin, etc ; hence the necessity of adding a certain
amount of those methylen compounds to the fusible saliretin-resin
before the mass is submitted to hardening or polymerization by
heat. The chemical reaction of the methylen compound on the fusi-
ble saliretin-resin is accompanied by the further elimination of water,
which can easily be demonstrated by direct experiments.

If hexamethylentetramin is used, an abundant liberation of
ammonia takes place at the same time ; but even with the use of the
latter, a certain amount of water is liberated by the action of the
hexamethylentetramin on tlie free phenol contained in the fusible
soluble saliretin-resin.

Barring those minor differences in preparation and proportions,
the final product "C" is practically the same as what is obtained by
the first or direct method as described above.

If hexamethylentetramin be added to the fusible resin, and heat
be applied, the violent exothermic reaction which ensues causes an
abundant liberation of ammonia gas. The mass raises. like bread,
and a hard spongy product is the result. Aylsworth^" utilizes this
foaming to prepare this substance in powder form by first producing
porous masses of the final condensation product, which can be
crushed more easily to a fine powder than if solid lumps of this
refractory material have to be pulverized.

In molding processes where high temperatures are needed, so as
to insure quick hardening, this violent liberation of ammonia gas
can easily be counteracted by suitable counter-pressure. In this
case, the pressure is not only, required for shaping the article, but
first and foremost, for avoiding porosity. This can easily be
demonstrated by heating the mass in an open mold, at the same
high temperature as is used in the press ; under these conditions,
direct application of these high temperatures causes foaming and
porosity, unless suitable counter-pressure be applied.

It has been claimed that by the use of hexamethylentetramin in
s" Aylsworth, Belgian Patent No. 240,116.

16 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

connection with perfectly dry fusible soluble phenol-resin, no water
is liberated, which is supposed to be an advantage for certain appli-
cations where high dielectric properties are recjuired. However, it
should be noted that such fusible soluble phenol-resins all contain
considerable amounts of free phenol and by the action of hexmethyl-
entetraniin on this phenol, water is formed besides the ammonia
that is set free.

Moreover, the presence of large quantities of free ammonia is,
if anything, more objectionable for certain purposes than the possi-
ble presence of small amounts of water.

It is true that free ammonia can be expelled by sufficiently long
after-drying of the molded articles, but by the same means it is just
as easy to expel the last traces of water. The most striking fact
is that there is no serious difficulty in obtaining articles of extremely
high dielectric properties, even when starting from raw materials
containing considerable amounts of water, provided the manu-
factured articles be submitted afterwards to a drying treatment,
which can be performed in any suitable drying stove.

It should be noted that almost all molded commercial articles
made of phenol-formaldehyde condensation products contain
various amounts of fibrous materials, preferably wood-pulp or
finely divided sawdust. These organic fibrous materials, at the high
temperature at which the molding in the hydraulic press takes place
(140° to 160° C. or over), begin to liberate variable amounts of
water and other products of decomposition, which depress the
dielectric properties. This is another reason why all molded articles
intended for purposes where high dielectric properties are essential,
should be submitted to oven-drying after they are molded. Those
who are unfamiliar with the technical side of the subject may ask
why it would not be simpler to omit altogether the use of fibrous
organic materials. They might suggest the use of asbestos. But
asbestos has other drawbacks, which limit its use. For instance,
asbestos is a relatively poor insulator, and the strength imparted by
its fibres is not so great as that imparted by vegetable fibre : fur-
thermore, its specific gravity makes the articles compounded there-
with very heavy ; moreover, any asbestos compositions which have
to be machined or milled are very severe on ihe tools. Another
objection is that asbestos compositions do not take the excellent and
easy polish which can so easily be developed on articles made with

PHENOL-FORMALDEHYDE CONDENSATION PRODUCTS 17

wood-fibre compositions, nor do they possess the elasticity and
strength of the latter.

It might also be suggested to drop entirely the use of any fibrous
material, and to use amorphous or pulverulent fillers. But the
technical requirements forbid this. Indeed, the main character-
istic of the final phenol-formaldehyde condensation products is that
although they are exceedingly hard and resistant, and have a
remarkably high crushing strength, their flexibility and elasticity
are very limited. In regard to these latter qualities, they occupy a
position between hard rubber and glass. A sudden shock or limited
bending shatters them, and this would restrict enormously their
technical applications. I found that the shattering wave induced by
impact could be considerably modified by the suitable introduction
of fibrous or cellular materials, like wood-fibre. This behavior is
quite different from that of other plastics like celluloid or rubber,
which lose their best and characteristic qualities by the incorporation
of filling materials. The phenol-condensation products, on the con-
trary, are enormously improved for commercial use, if compounded
with filling materials, provided the latter be of a fibrous nature ; in
the latter case, they lose their natural brittleness; can stand shock
and impact, without shattering; they can be rendered flexible and
yet maintain all their other excellent properties of high resistivity
to physical and chemical agents.

Hence, some of the most important industrial applications of
these condensation products are precisely those where they are
used in conjunction with fibrous bodies ; for instance, they serve to
impregnate fibrous materials like wood, pulp-board, and to indurate
the latter, or to agglutinate firmly loose fibrous substances, like
wood-fibre, or fine sawdust, which then act as a structural skeleton
distributed throughout the indurated mass.

This important technical result is easily demonstrated by com-
paring the enormous strength and resistance to impact or shock of
molding compositions containing wood-fibre with others containing
the same amount of structureless filling materials, for example,
powdered materials. Compositions made with the latter will be
found incomparably more brittle and very much less appropriate, if
not entirely unsuitable for most industrial purposes, and more
especially for molded articles where great strength is required.

Other important technical results are accomplished with the use

18 AMERICAN INSTITUTE OF CUEMICAL ENGINEERS

of filling materials ; for instance, the highest dielectric properties
have been rendered possible by the joint favorable action of fibrous
material and heat and pressure.

It might be cited here that paper impregnated with these con-
densation products, and submitted to hardening under heat and
pressure, has made it possible to manufacture sheets which show
an astonishingly high disruptive test (puncture lest), averaging
77,000 volts a. c. on sheets on one-sixteenth of an inch thick, corre-
sponding to 1230 volts per mil or about 48,500 volts per millimeter.

Under these favorable conditions, the vegetable fibre of the
paper is thoroughly impregnated with the condensation product,
and the high pressure has excluded the possibility of porosity
induced by foaming.

PROTECTION OF INTELLECTUAL PROPERTY IN
RELATION TO CHEMICAL INDUSTRY

By President I., n. IJAEKELAND

Read at the Detroit Meeting, December 4. 1912.

The mass of unthinking people, as well as those whose views
are predominantly guided by precedent, have little or no conception
of the natural rights of intellectual property. It is difficult to teach
such people that adequate protection of intellectual property is
abundantl}' more beneficial- to the community at large than to the
temporary individual possessors of these rights.

Yet these same people consider as sacred and inviolable any
other property rights as soon as the latter relate to chattels or real
estate, whether such rights were obtained by purchase, by inheri-
tance, by gift, by privilege, by labor, or in any other way.

Furthermore, the laws of all nations are very strict in protecting
such property rights, but do not concern themselves beyond certain
limits, whether the possessor of the property is morally entitled to
it or not. Neither do our laws concern themselves whether the
owner uses his property for good or for wrong, for the benefit of
the community at large, or for the gratification of his own selfish
purposes. From the standpoint of the law (with very few excep-
tions, such as, for instance, Board of Health or police ordinances,
or cases of so-called eminent domain), it matters little whether the
private ownership of some property is a burden to the community
or whether it is an impediment to the happiness or the free develop-
ment of its citizens.

Neither is there any disptite as to the time the ownership of
such property should last. Except for restrictions put on ownership
by taxes, property rights are practically perpetual, and can only be
transferred by accepted methods, as, for instance, sale, barter,
inheritance or donation.

In some rare instances, there may be expropriation for public

19

20 AiIERJCA.\ INSTITUTE OF CHEMICAL ESGISEERS

purposes (or eminent domain), but even then, some suitable com-
pensation is usually made.

All this is readily accepted as an axiom, as an underlying article
of faith by all laws relating to property. Only the socialist dares
dispute these rights, while even the single-taxer admits them to
such a decided extent that he desires to abolish taxes on all property
created by labor or enterprise, so as to shift the burden of all
taxation on unearned land values.

When, however, it comes to recognize the claims of ownership
to intellectual property, the result of the truly creative effort of the
citizen, we butt right away against some stubborn conceptions,
Vk^hich have petrified into the code of our long-established laws.

If Tom steals Dick's two-dollar scarf-pin, Dick will have little
trouble in putting Tom in jail, even if Dick himself has obtained
his pin by questionable methods. But when it comes to protecting
even for the short period of seventeen years, the most logical, the
most legitimate personal property, intellectual property as embodied
in patent rights, with all that it involves, with enterprises depending
thereon, based often on the work of a lifetime, then our law courts
are woefully deficient, on account of the uncertainties, delays and
enormous expenses connected with the adjudication of patent
rights. All this works overwhelmingly in favor of the litigant with
the well-filled purse, the large corporation.

Yet no country in the world has expressed in a fairer and
broader spirit the rights of intellectual property than the United
States, in Article I, Section 8, of the Constitution: "Congress shall
have power to promote the progress of science and the useful arts by
securing for limited times to authors and inventors the exclusive
right to their respective writings and discoveries."

This proclamation lifted the right of a patentee at once far
beyond the mere privilege conferred by most other countries, which
grant patents not only to the real inventors or originators, but also
to those who are first to introduce unpublished inventions into their
respective countries. With some legitimate pride, we can say that in
this respect at least, American patent law stands head and shoulders
above the laws of Germany, France and England.

The principles of the right of intellectual property so clearly
defined in our Constitution, were repeated in the preamble of the
French Law of January 8, 1791. which declares:

^PROTECTION OF INTELLECTUAL PROPERTY 21

"The National Assembly, considering that every new idea,
whose manifestation or development may become useful to society,
belongs to him who conceived it and that not to regard an industrial
invention as the property of its author would be to attack the
essential rights of man ; considering at the same time how much
the lack of a positive and authentic declaration of this truth may
have contributed till now to discourage French industry by occasion-
ing the emigration of numerous distinguished artists and by causing
to pass out of the country a great number of new inventions from
which the Empire ought to have drawn the first advantages ; con-
sidering finally that all the principles of justice, of ptiblic order, and
of national interest imperatively command that it determine for the
future the opinion of French citizens with regard to this class of
property by a law which consecrates and protects it, . . . etc.''

The wisdom of these provisions has been abundantly proved by
subsequent events. Only a man stubbornly blind to evident facts
will deny that just those countries which have the most liberal laws
for patent protection, are also those which have taken the lead in
the industrial and scientific development of the world. No man was
more imbued of the benefits of the patent system than Abraham Lin-
coln, when in i860, in his speech at Springfield, Illinois, he said:

"In the world's history, certain inventions and discoveries
occurred of peculiar value, on account of their great efficiency in
facilitating all other inventions and discoveries. Of these were
the art of writing and of printing, the discovery of America, and
the introduction of patent laws. . . . The patent system . . .
added the fuel of interest to the fire of genius, in the discovery and
production of new and useful things."

Up to about thirty years ago, our patent system covered tolerably
well the purpose for which it was intended. It stimulated individual
inventions and promoted numerous private enterprises. Since then,
with the extraordinary growth of our nation, with the tremendous
increase of agglomerations of capital for industrial enterprises, and
more specially with the astonishing increase in the ramifications of
applied science, our patent system has become totally inadequate
to the needs of the country ; it suits our new conditions in about
the same way as baby clothes fit an overgrown boy.

Our patent system, although based on an excellent fundamental
law, has now degenerated into a set of exceedingly complicated

22 AMEKIC.iX ISSTITUTE OF CHEMICAL ENGINEERS

technicalities of law practice, a system of legal acrobatics, whereby
any contestation before the courts can be turned into "perpetual
motion" to the advantage of wealthy litigants, and whereby the
individual patentees of slender means and the small industrial con-
cerns, tlnd themselves under smothering disadvantages when oppos-
ing rich antagonists. In this way our patent system, instead of
accomplishing its intended purposes of stimulating individuality,
simply reinforces the rich and big industrial enterprises, and dis-
courages the individual inventor unprovided with a liberal bank
account.

I shall not take up your time by repeating all that has lately
been published on the subject, but refer you to the available printed
publications: Abuses of our Patent System, L. H. Baekeland,
Journal of Industrial and Engineering Chemistry, \'ol. 4, p. 333,
1912; The Incongruities of Patent Litigation, ditto. Vol. 4, No. 11,
November, 1912. The United States Patent System, Robert N.
Kcnyon, Transactions of the American Institute of Chemical
Engineers. Vol. I\', 191 1. The Gist of the Supreme Court Decision
in the Dick Patent Case, and of the Proposed Law Amendments,
Gilbert H. Montague, The Engineering Magazine, May-June, 1912.
The Sherman Anti-Trust Act and the Patent Law. The Supreme
Court on Patents (the Dick Patent Case), Gilbert H. Montague,
Yale Law Journal, April-May, 1912. Report No. 1161, to accom-
pany H. R. 23,417, August 8, 1912, Hon. W. A. Oldfield, Chairman
of the Committee on Patents, Washington, D. C.

It is true that on November 4, 1912, the Supreme Court of the
United States promulgated revised Rules of Practice for the
Courts of Equity, which intend to simplify our methods of litiga-
tion. Unfortunately this is only a half-way measure, leaving still
abundant opportimity for the tactics of delay, chicane, and expense
which have too much disgraced American patent litigation.

These new rules might gain in efficiency, if they were supple-
mented by the creation of a final court of patent appeals. They
might be made incomparably more efficient if they could be
strengthened by a system w'hereby the adjudication of the validity
of patents does no longer devolve upon judges who do not possess
the technical or scientific preparation required nowadays for dis-
cerning the merits of complicated patent questions. Some of the
far-reaching details of scientific technology absolutely baffie the

PROTECTION OF INTELLECTUAL PROPERTY 23

comprehension of those who have no preliminary technical or
scientific training. Certain problems of chemistry and physics
involved in many patent suits can no longer be understood by an
intelligent judge, if he has not had long and systematic preliminary
training in that branch of knowledge. I do not deny that an intelli-
gent judge can be coached and instructed by long, tedious, time-
robbing methods, even in intricate scientific problems ; but his edu-
cation has to be made over again for each special case. After you
have made a chemist of him for one case, the next adjudication will
require the knowledge of a physicist, an electrician, an engineer,
and so forth.

What would any judge say of a chemist or a mathematician,
or an engineer, totally ignorant of the practice of law, who tried
to conduct a law case in court? Such an amateur lawyer might
succeed in doing so, but to what hopeless loss of time, misunder-
standings and confusions .would this lead before the subject had
been mastered to some extent? Yet this is exactly what happens
with a judge to whom we entrust to decide on the validity of a
patent involving highly intricate scientific or technical subjects.

Judge Hand expressed himself very eloquently on this
subject:

"I cannot stop without calling attention to the extraordinary con-
dition of the law which makes it possible for a man. without any
knowledge of even the rudiments of chemistry to pass upon such
questions as these. The inordinate expense of time is the least of the
resulting evils, for only a trained chemist is really capable of passing
upon such facts, e.g., in this case the chemical character of \^on
Furth's so-called 'zinc compound,' or the presence of inactive organic
substances. In Germany, where the national spirit eagerly seeks
for all the assistance it can get from the whole range of human
knowledge, they do quite difl^erently. The court summons technical
judges to whom technical questions are submitted and who can
intelligently pass upon the issues without blindly groping among
testimony upon matters wholly out of their ken. How long we
shall continue to blunder along without the aid of unpartisan and
authoritative scientific assistance in the administration of justice,
no one knows ; but all fair persons not conventionalized by provin-
cial legal habits of mind ought, I should think, unite to effect some
such advance." (See Parke-Davis & Co. z'S. M. K. Alulford Co.,

24 AMERICAN ISSTITUTE OF CHEMICAL ESCISEER.'i

Circuit Court, Southern District of New York, April 28, 191 1, 189
Federal Reporter, 95.)

Even under the new rules it will not be difficult to drag on a
case by presenting an unrestricted amount of testimony taken
before an incompetent examiner and by calculating every step so
as to tire out your opponent, and so as to lead the judge into doubt
and error, by swamping him with endless contradictory expert
testimony calculated to befog the issue instead of making it clear.
Such tactics are relatively easy for the litigant who, for that pur-
pose, can afford to pay accommodating experts and skillful lawyers.
Even if at the end the judge, after laborious and conscientious
efforts, masters the technicalities of the case and reaches a good
decision, much needless time has been wasted. All this might
easily be avoided, and judges might be saved the trouble and
responsibility of going in every single case through a different
scientific or technical training, if their intervention could be limited
to what they are competent for, namely, to detemiine what claims
have been infringed and in how far this infringeinent entitles the
patentee to damages.

That such a method of settling patent suits is quite practical,
is shown by the example of Germany. In that country patents are
allowed after preliminary examination, just like here ; but, after
the patent is granted, it can be attacked for annulment or revoca-
tion before a competent court in the Patent Office. So that any
party who is sued for infringement of a patent which he thinks is
invalid, can avoid temporarily the adjudication of the infringement
issue by starting an annulment or revocation suit. In the mean-
time, the courts in which infringement cases are examined have to
take the patent as it stands, and it is only left to them to interpret
the scope of the claims, and to what extent these claims have been
infringed.

This relieves the equity court of all the complicated questions of
validity or non-validity of a patent, and puts the whole matter in
the hand of a properly constituted court of experts, who can handle
this subject with incomparably less hesitation or delay. Besides
this, the whole system of practice in the German Patent Office
tends toward systematic elimination of invalid patents. After an
examiner has decided upon preliminary allowance of a patent, the
claims and specifications are open for public inspection, and for a

PROTECTION OF INTELLECTUAL PROPERTY 25

period of two months anybody whomsoever can file arguments
against the final grant of the patent. In this way, the nation does
not confer too lightly patent privileges and has, furthermore, the
benefit of the free advice of any experts in the art. who may advance
good reasons for non-allowance of the claims, of which the
examiner was not aware when he rendered his first decision.
These opposition proceedings give added thoroughness to the work
of the examiners. They are relatively inexpensive and do not
necessitate the intervention of law counsel. Sometimes they delay
the issue of a patent, if there is any good reason for doing so.
On the other hand, a patent that has successfully withstood vigor-
ous opposition proceedings is very much strengthened thereby.
This, in itself, is a very valuable compensation for any delays to
which the patentee may have been subjected. In other words, by
that system, a good patent becomes stronger, while a defective
patent application is easily weeded out. A similar system of public
opposition exists here in the United States in relation to the grant-
ing of trade-mark rights, and seems practical enough to be extended
to our methods of allowing patents.

Such a sifting process, first by the examiner, then by opposi-
tion proceedings, sometimes by annulment or revocation proceed-
ings, for wrongly issued patents, involves no serious difficulties
nor great loss of time if carried out by courts of experts. Thanks
to such a system, the work of a judge who acts on an infringement
case, gains considerably in dignity and is, at the same time, enor-
mously shortened and simplified. ( See Wertheimer, The German
Patent System, Electrical World, May i8, 1912.)

The German system throws the burden of technicalities and
expert knowledge on the Patent Office, or the courts connected
therewith. Nothing would be easier than to introduce a somewhat
similar system in our country.

All officers of our patent office, high or low, should be made
independent of any political favoritism ; they should be better paid,
with more opportunity for promotion, according to merit ; their
w-ork should be made simpler by an improved office equipment and
increased facilities for a thorough search ; furthermore, our
unnecessarily complicated and expensve methods of interference
proceedings should be simplified.

With these reforms, there is no doubt that we can organize right

26 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

in the Patent Office, a competent court, supplemented by the court
of appeals of the District of Columbia, for deciding in a very
expedient way all questions of validity of patents.

This court of appeals, because it is situated right in Washington,
would have easy and immediate access to all the records of the
Patent Office; by this fact alone, it would have superior opportuni-
ties for prompt and efficient work.

During recent years, Germany has been trying to broaden its
patent laws more and more towards the principles set forth in the
American Constitution. For instance, it has practically eliminated
the system of compulsory licenses except in some rare instances
where public welfare is involved. If only we could borrow some
of the more efficient methods with which the German patent law i.s
administered, and enforced, we might succeed in making an Ameri-
can patent real property for poor and rich alike, instead of a pretext
for expensive and endless litigation, with all the advantages it gives
to the richer litigant, to the detriment of the consumer, who in the
end pays the bill.

At least some of these facts seem to have been very well recog-
nized in the masterly report of Hon. William A. Oldfield, chairman
of the House Committee on Patents. (See report No. 1161, on
H. R. 23,417, August 8, 1912.)

Unfortunately, his proposed Oldfield Bill (H. R. Xo. 23,417),
with a regrettable lack of consistency, neglects utterly the para-
mount issues, and busies itself with secondary regulations, which, if
carried out, will practically put a penalty on patented articles.

The new provisions of the Oldfied Bill aim at curtailing the
power of patents in the hands of trusts or large corporations : but,
in doing so, new provisions are introduced which will create end-
less new opportunities for protracted litigation.

The Oldfield Bill overlooks the axiom that whatever increases
the expense or delays of litigation is a very potent weapon in the
hands of large corporations, which they can hurl against the poor
litigant who stands in their way.

The saddest thing of all is that the new Oldfield Bill tries to
abrogate the hitherto accepted principle established by our Consti-
tution, that the patentee has the right to license or sell his patent
on whatever terms he pleases. It has been feared that this princi-
ple, if carried too far, might become a dodge for avoiding anti-

PROTECTION OF INTELLECTUAL PROPERTY 27

trust laws. Since the decision of the famous, but harmless, Dick
case, the most hysterical exaggerations have been published on this
subject. Fortunately, since then, the recent and unanimous decision
of the United States Supreme Court in the "bath tub trust" case,
November i8, 1912, does away with all these redundant arguments
and settles, beyond doubt, the principle that, patent or no patent,
vmlawful combinations in restraint of trade can be stopped by the
Sherman Law.

The Oldfield Bill, in its eagerness to avoid any hesitation on
this subject, goes one step further, and unfortunately, one step too
far. It puts so many restrictions on the sale of a patented article, or
on a patent license, that it may become a positive disadvantage to
transact business by means of patents.

Examined in its last analysis, it threatens a business based on
patented processes or patented articles, with penalties which
unpatented articles are thus far not subjected to. It takes the
proposed patent law as a pretext for saddling a patented article
with restrictions which have not heretofore been formulated for
non-patented goods.

This unexpected paradox, promoted by the Oldfield Bill, is dis-
tinctly in opposition to the rights of intellectual property conveyed
by the words and the spirit of the Constitution, and if the Oldfield
Bill becomes an effective law, it will be the saddest blow ever given
to our patent system. It will do comparatively little harm to large
business interests, because for them, there are many ways of cir-
cumventing its provisions; on the other hand, it will cause great
discouragement to smaller enterprises which until now have held the
hope of matching inventive genius and initiative against the money
power of big organizations. Make a large corporation respect the
patents of a small concern, or of an individual, and you reduce at
once any advantage of size or money power, and at the same time,
you encourage the most beneficial form of competition, competition
based on improvements. But to introduce curtailing restrictions
for the licensing or selling of patented articles or patented pro-
cesses to which non-patented articles are not subjected, means
simply obliterating the value of patents while needlessly increasing
still further the opportunities of endless and ruinous litigation and
chicanery.

Another unfortunate miscarriage of purpose in the Oldfield Bill

28 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

is its provision against so-called wilful "suppression" or "non use"
of patents. It does not take into consideration that in numerous
instances, a patentee or an assignee possesses a series of so-called
alternative patents, which can be used to bring about identical or
similar technical results by modified means. Among such alternate
patents, the best or the most suitable is used, absolutely irrespective
of any other reason or intention to suppress their use. Yet without
the exclusive possession of every one of these patents, the inven-
tion would not sufficiently protect against competitors, and
the field would be so much reduced as not to make it worth while
to put one's best energies to the development of the invention. In
most cases, it would become a material impossibility for a small
concern to maintain the exclusive ownership of its patents, if it
had to go to the enormous expense of working simultaneously all
its "alternate" patents ; by omitting this expensive technicality, it
would be exposed to the risk of being compelled by its competitors
to grant a compulsory license ; this would practically annihilate the
advantage of exclusive ownership as expressed by the Constitution.
Here again large concerns would be at an overwhelming advantage
because they can at an expense relatively small for them, equip
the necessary appliances for remaining within the technical pro-
visions of the law. In the meantime, they could easily harass their
financially weaker competitors by exacting from them compulsory
licenses which would break up the only prospects of successful com-
petition which the smaller concern might have possessed, until then,
in its patents.

In other words, the Oldfield Bill is aiming at the petty side of
the situation, and in doing so, has unwittingly picked out a vital
spot of our patent system. It reminds one of the man who set his
■barn on fire in order to drive out a hornet's nest.

I have no doubt that this bill has been framed with the best inten-
tions for the interests of the country. Unfortunately, the framers of
this bill do not foresee the far-reaching and dangerous effects of
its provisions.

The average man, even the average legislator, has a rather one-
sided conception of patents or inventions. Most people's idea of a
patent does not go far beyond some simple mechanical device, like
a patented mole-trap, a safety razor, an alarm clock, or other simi-
lar invention, more or less easy to understand after the apparently

PROTECTION OF INTELLECTUAL PROPERTY 29

simple mechanical principles have once been explained. Then
everything seems so simple and easy to them, that their limited
imagination cannot conceive how even these apparently simple
devices have frequently cost incredible efforts and immense amounts
of money before their advantages become available to the
public.

This attitude of mind develops, naturally, the belief that a pat-
entee has a "soft snap," the result of a lucky idea, in about the
same way as a lucky prospector strikes a rich gold mine, or a lucky
ticket draws the grand prize in a lottery.

Precisely on this account, it becomes difficult to explain to such
people the rights and purposes of intellectual property ; it is still
more difficult to convince them that the nation is greatly benefited
by liberal patent laws.

When it comes to chemical patents, the ignorance of the average
public is amusing if not pathetic. Since we have heard a New
York alderman in an official address of welcome to the members of
the International Congress of Chemistry speak as if they were
druggists or pharmacists, we must no longer be astonished if the
average Congressman or Senator refers to a chemical patent as a
synonym of "patent medicine."

But it is even difficult for the better prepared legislators, to
understand how some chemical inventions have brought about the
most far-reaching developments, not only in other industries and
arts, but in civilization itself.

For instance, it is not so obvious to them how processes for
fixing the nitrogen of the air, or extracting soluble potassium salts
from rocks, enable us to make food supplies independent from the
restricted potash mines in Germany or the nitrate deposits in Chili.
Such inventions are no more nor less than a means for preventing
possible starvation of our race. Do they realize that the develop-
ment of the automobile, with all that it directly and indirectly
implies, was entirely dependent on Goodyear's vulcanizing process
of rubber? Shall we remind them of the fact that without the
invention of explosives, like dynamite, gigantic engineering enter-
prises, the Panama Canal, blasting of rocks for the excavation
of our cities, mining for ores, tunneling and grading of railroads,
would be impossible ? How could we expect even the most per-
fected modern printing presses to distribute to every citizen, rich

30 AMERICAN INSTITUTE OF CUEMICAL ENGINEERS

or poor, young or old, that knowledge and culture, which means
belter citizenship, better opi)ortunities for happiness and develop-
ment of our race, if it were not for the inexpensive and abundant
supply of paper furnished by the cellulose processes. The Greeks,
the Romans, and even the Middle Ages, had their sages, their
poets ; yet those were the times of slavery and oppression, because
knowledge was only in the reach of such a limited number that it
was possible for tyrants to tlirottle its diffusion by sending the few
advanced thinkers to the gallows or burning them alive. For the
same reason, scarcity of books, the destruction of the library of
Alexandria, was a calamity for the intellectual development of
mankind. Our abundant supply of cellulose makes a repetition of
such conditions an utter impossibility.

Then again, where would we find our supplies of steel, the main
raw material for modern engineering, if the Bessemers, the
Thomas-Gilchrists and others had not invented their processes?
How about the marvelous synthesis of products derived from coal
tar, which liavc literally created the most astounding series of new
substances which have revolutionized therapeutics, surgerj', hy-
giene, and are finding daily new applications in the most varied arts
in general technology ?

At a time when all countries are confronted with tiiat critical
question of the increased cost of living, it may be interesting to point
out that just those industries where invention and patents have
played the smallest role, are also those where the increase of price is
most burdensome, while those commodities where patented inven-
tions have had the fullest influence, have, on the contrary, decreased
in price, and in some instances, to an astonishing degree.

For instance, the price of sulphuric acid is about fifteen times
less than it was in 1807, and about one-half of that of 1870. The
price of soda ash is about one-sixth of what it was in 1823, and
about one-half of the price in 1S60. Nitric acid sells for less than
one-half the price of 1861. Glycerine sells for about one-eighth
of the price of 1855. Chloride of lime in 1800 sold for 30 cents a
pound, in 1870 for about 2 cents per pound, to-day for about i cent
a pound. Any chemist knows that every one of these products is
used directly and indirectly in the most ramified channels of our
arts and industries, but the layman does not know that cheap soda
means cheap soap, cheap paper, cheap glass, etc., that cheap sul-

PROTECTION OF INTELLECTUAL PROPERTY 31

phuric acid means cheap fertilizers, better crops, cheaper corn,
cheaper wheat, and so forth.

Let me point out that the decrease in price of these materials
is even considerably greater than the bare comparison of figures
indicates, if we take into consideration that the purchasing value
of money has considerably decreased, while the cost of labor has
enormously increased.

Nor are these examples merely confined to chemical products.
The reduction in price for articles where patents have played an
important role is just as evident in steel products, tools, machinery,
etc.

Compare these lower prices with the vastly increased cost of
rents, clothing, foodstuffs and many agricultural products, where
patents have played a less preponderant role. If you will carry your
analysis still further, you will find that in such branches of trade
where patented inventions have had little or no importance, for
instance, cattle raising, prices have soared highest. On the other
hand, for such agricultural products where patented machinery
could be used to best advantage, like wheat and corn, the increase
of price has been relatively small. Then again, garden vegetables,
potatoes, etc., where the use of patented agricultural machinery is
less available, show an enormous increase in price. .

You may object that the price of shoes has gone up, but here
again, the increase is entirely due to the greatly advanced price of
hides, and were it not for the perfected shoemaking machinery,
and for the better and cheaper chemical tanning methods, all due
to patents, the cost of our shoes would be so high that they might
again become an article of luxury, available only for the well-
to-do.

The present price of clothing is high enough as it is ; neverthe-
less, it would still be much higher but for the patented machinery
for spinning and weaving, the patented chemical processes of
bleaching, dyeing, mercerizing, etc.

I should not omit to mention our vastly improved and cheaper
methods of transportation, of production of power and light, all
developed and perfected on an interwoven system of patents. I
could explain the far-reaching influence thereof on civilization,
culture, on the happiness and security of life of the individual citi-
zen ; but even then I might not convince the pessimist or the

32 AMERICAN IXSTITLTE OF CHEMICAL ENGINEERS

scoffer, who only sees the hole in a doughnut and stubbornly per-
sists in ignoring the doughnut itself.

The history of almost every invention which we are utilizing
now, unconsciously, every day, is an epoch by itself, the details of
which are only known by the few pioneers who gave the best they
had to give, who helped with their brains, with their money, and
talent of organization ; some with their very lives.

The oft-repeated statement has been made: "An inventor can-
not help inventing, whether you give him a reward or not." Then
again, some others say: "Necessity is the mother of invention."

The most apparent fact is that the man who receives an ample
income from his father, or some other privileged source, is less
prompted to distinguish himself by arduous creative work on inven-
tions than the poor but intelligent man who sees in invention a
means of making himself financially free and independent, as well
as giving an outlet to his inventive abilities.

Whoever has followed intimately the development of some
chemical processes knows very well that whether "the inventor
cannot help inventing," or whatever may be the incentive to inven-
tion, most of these important inventions could never have been
carried out, or could never have been brought to the point where
they became of public benefit, but for the intelligent use of vast
sums of money. Too few people have a conception of the immense
sacrifices, of the serious money risks, involved in the development
of some patents. Many chemical inventions used now currently
and open to the public at large, have cost millions before they were
brought into practical shape, or before the public was educated to
their advantages. Can any one e.xpect that such expenses, such
efforts, such risks, would be undertaken, unless there was the pos-
sibility of at least some chance of recouping by a temporary patent
protection ?

Let us take, for instance, those large German chemical com-
panies, which employ hundreds of chemists and engineers, engaged
exclusively in research work; to them we owe the development of
many processes which have had an untold beneficial influence in
many directions on the economics of our daily life, even on civili-
zation itself. They employ large aggregations of capital, reaching
into many millions. The dividends of some of these companies
may appear large to the superficial observer. Yet if you look more

. PROTECTION OF INTELLECTUAL PROPERTY 33

closely into it, you will find that these very companies were founded
long ago, some of them over half a century or more, that the large
capital which they employ has never been "watered," that although
they have had the benefit of the devoted cooperation of an endless
number of distinguished men, stars of first magnitude in their pro-
fession, the net returns on their invested capital, at the end of half
a century of brilliant intellectual pioneer work, is relatively small,
even if the dividends seem large. In fact, the net returns are
decidedly lower than that of many American enterprises not over
fifteen years old, and where progressive technical leadership was
entirely larking, but where tariff privileges and agglomeration of
competing concerns into a trust insured a splendid paying monopoly,
notwithstanding the reckless financiering of their promoters.

If you will further investigate the history of those German
chemical concerns which have become leaders of the industrial
world by nothing but their intellectual pioneership, you will find
that, notwithstanding all the patents on which they have to rely,
the expenses involved in research work and pioneership, swallow
up, to a large extent, the profits realized in some of the established
branches. But with true scientific spirit, their far-sighted directors
were willing to sacrifice a very considerable part of their earnings,
in their search for improvements and development of new ideas;
they have set a magnificent example in the only competition bene-
ficial to the public, competition by improvement.

One of our wealthiest retired multi-millionaire manufacturers,
not so long ago, speaking about his money successes, gave the fol-
lowing advice: "Never be a pioneer; it does not pay. Let the
other man do the pioneering, and then after he has shown what
can be done, do it bigger and more quickly; but let the other man
take the time and the risk to show you how to do it." To anyone
who advances the statement that an inventor "cannot help invent-
ing," I desire to ask whether an inventor will do much inventing,
if in order to carry on his research work, or to develop his invention,
he has to spend hundreds of thousands, nay sometimes millions of
dollars, but does not possess them, and nobody is willing to take the
risk to furnish the money unless there is a fair chance for his
backers of obtaining some compensation by a temporary patent
protection? Those who know the large sums of money which have
been swallowed up by the research and development work con-

34 AMERJCAX ISSTITLTE OF CHEMICAL ESCISEERS

nectcd with the artificial production of nitrates; with the Solvay
soda process ; the development of the steam turbine ; electric light,
electric traction, and numerous other inventions of far-reaching
magnitude, will know what I mean.

Just on this account, it is highly unreasonable of the Oldfield
Bill to try to make a distinction between the inventor in whose
name the patent is drawn, and the party who runs the risks in
enabling the inventor to make the invention available to the public.
Any such legislation simply tencls to discourage those who, at con-
siderable risk, furnish tlie capital and the talent to develop an inven-
tion into a commercial possibility, and who thereby bring it into real
public service.

Now and then, I have perceived that some of my fellow
chemists, who. although highly trained, have never created any-
thing of technical value, and whose experience with matters of
practical life frequently does not extend beyond the confines of their
lecturerooin or their laboratory, do not seetn to grasp fully the
immense distance that lies between the initial conception of an inven-
tion, or its study in the laboratory, and the overwhelming amount of
careful work and money risks connected with its development on a
commercial scale, until it has safely reached the point where the
public can avail itself of the invention.

I wish to cite, for instance, the famous Solvay process, which
gives us cheap, excellent and abundant soda, an article of prominent
importance in the wheels of our civilization. This process was
known and described more than a dozen times, and had even been
tried repeatedly at considerable loss, on a commercial scale, many
years before Solvay tied his genius to this difficult problem and
developed from an unreliable laboratory reaction a process of
great industrial importance ; then, with a staff of able collaborators,
and the employment of large amounts of cash, he overcame, by and
by, the technical drawbacks which had caused the failure of all of
his predecessors.

Hundreds of similar examples could be cited. Whoever has
been intimately acquainted with the commercial development of
some of the most successful inventions, knows quite well the risks,
dangers of failure, which have accompanied the herculean task of
development and educational work. It is a well established fact that
the great majority of new enterprises fail, that few succeed.

PROTECTION OF INTELLECTUAL PROPERTY 35

The educational effect due to the introduction of patented inven-
tions is of immense benefit to the pubhc, although this fact is not
very apparent to most people. In many instances, the owner of a
patent frequently has to go to extreme sacrifices before he succeeds
in convincing the public of the merits of his invention ; in fact, the
public stubbornly refuses to benefit by an improvement to which it
has not been fully educated.

The practical value of cash registers only became obvious after
a most thorough and very expensive educational campaign.

The metric system is just as useful as the cash register ; it was
invented long ago and systematized in all its details during the first
French republic. Nevertheless, to-day there are still two large com-
mercial countries, the United States and England, which have not
yet been educated to its merits ; if the metric system had been
patented, like the "cash register," somebody, during the seventeen
years of the patent monopoly, would have undertaken the money
risk and arduous task of thoroughly explaining the advantages of the
metric system to our conservative citizens, and we would have
ceased long ago to submit to the burden of waste of time and
money caused by our antiquated, cumbersome system of weights and
measures.

It has been stated, with much reason, that the best way to post-
pone the benefits of an invention is to allow public use of a patent,
because then nobody takes the risk of starting an educational cam-
paign or of developing the invention, which, after all, means pull-
ing the chestnuts out of the fire for the benefit of others.

Entirely new industrial enterprises are not easily started on
inventions which are not patented, unless some other method is
available for insuring some kind of a monopoly ; for instance, by
maintaining secrecy or by acquiring special skill, or by controlling
the raw material, or by tying the market, or in other instances
where the initial outlay for a plant requires a capital so large as
to exclude others.

Moreover, if you scrutinize those industries where secrecy of
methods, instead of published patents, is the prevailing tendency,
you will find that the secret-process-industries are precisely those
which have least progress to record, and where high prices rule.

Whoever desires to get posted on the modern literature pertain-
ing to any industrial chemical processes, will find that available

36 AMERICAN ISSTirVTK Of CHEMICAL ENOlHttlCi

text-books arc many years behind in information as far as novelty
and accuracy are concerned ; for this reason alone, it is absolutely
indispensable to get acquainted with all recent patent literature.

Were it not for the comi)ensation expected from patent rights,
most of this information would be carefully kept secret, or if it
were divulged at all, this would mostly occur by accident. Every
newly published patent sets to work the thinking cells of numerous
inventors, who are not slow to suggest further possible improvements.
Every patent of some importance is rapidly followed by a succes-
sion of other patents conceived by other inventors, who were
inventors, who were inspired by their predecessors, and so the
work of progress goes on unceasingly and at a quickened pace.

In the age of the alchemists, there were no patents ; inventions
and discoveries were jealously guarded and buried with their origi-
nators, and the world and its inhabitants remained very much what
they were, with most rights and comforts in the possession of those in
power, and very little chance of improvement for the non-privileged
classes.

The public should be educated in these truisms. Unfortunately,
the education of the public has been directed in the opposite way
since patent infringers have utilized the daily press after the late
decision of the Supreme Court in the Dick case, to start a cam-
paign for urging our well-meaning but ill-prepared legislators
towards patent reform, which will give still broader scope to our
modern buccaneers. This reminds me of the man who, after steal-
ing a stranger's pocketbook, kept on shouting "stop thief," so as to
distract the attention from himself.

Two ways are open for our legislators:

One way is to try "to hit the trusts" by mutilating the best there
is in our patent system, which has been such a potent factor in the
development of our country; to chill the best incentive for private
enterprise ; to stunt that kind of competition most beneficial to the
public, competition by improvement, incomparably better in this
respect for stimulating industry, science and progress, than pro-
tective tariff privileges which, in many instances, have worked in
the opposite direction.

The other way is not to put dangerous restrictions on the patent
rights defined by our Constitution. If there lias been any fear
that such patent rights might be abused for evading the provisions.

PROTECTION OF INTELLECTU/U PROPERTY 37

of the anti-trust laws, these apprehensions have vanished by the
clear unequivocal decision of the Supreme Court in the Bath Tub
case.

But there is urgent need of reform in our patent system by sim-
plifying procedure in the Patent Office as well as in the courts, by
insuring better, quicker and less expensive means for adjudicating
the title and validity of patents. Only such a reform will bring
about that, big or small, poor or rich alike may be stimulated by
the advantages of our patent system, instead of making a patent an
expensive but powerful instrument, available only to the wealthy.

Whatever simplifies and lessens the cost of the administration
of our otherwise excellent fundamental patent law, gives the enter-
prising man with small means a better chance of competition by
inventive progress and merit against ponderous aggregations of
capital. By such reform, which insures such healthy competition,
the nation is sure to be benefited.

In all above considerations, my remarks were principally
inspired from the standpoint of chemical patents, not alone because
this very important class of patents is least understood by the
average public and the legislator, but because chemical process pat-
ents are also those which are most difficult to protect from
infringers.

Discussion.

V.-Pres. Whitaker: We have all heard the earnest and masterly
address of our President. I think, as a rule, presidential addresses
are not discussed, and usually for obvious reasons, but I think here
is something in which we are all very much interested, and we
should be very glad to have additional remarks and questions, if
such occur to you in connection with this interesting subject.

Dr. Ittner: This patent question is a complicated one, and I
confess that I do not feel competent to suggest the improvements
that seem to be necessary — not nearly so well as Dr. Baekeland,
because he is in a position to recognize things better than I am. I
have seen the patent situation from perhaps a little different point
of view from that which Dr. Baekeland has dwelt upon, although
he has probably seen it from this point of view also.

I think that real inventors should certainly be protected in
the rights to their discoveries, and that the right to intellectual

38 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

property should be respected. Now, I tliink that a person has a
right to intellectual jiroperty, whether he makes that intellectual
property public knowledge or whether he keeps it secret. There
are some people who seem to think that whenever a thing is kept
secret that the knowledge is piracy, but it is not always piracy,
because the fact that it is pirated is evident in a product that is
turned out, and sometimes in the product that is turned out there
is no evidence of the process which is used, and for that reason
there are some concerns who believe that they get better protection
by keeping their processes secret, and 1 think that they have a per-
fect right to do so, and I think when they have property which they
have developed themselves they have as much right to that prop-
erty as those who make their property or their processes public
knowledge. I think there should be some way of protecting those
who have such processes, from being deprived of that right by those
who come along later and possibly by delving into their secrets
obtain those processes and even try to deprive them of their right
to carry out the processes which they have discovered.

When a man discovers something new he does not know all the
possibilities of it, of course. He may get some great principle which
is new and very valuable and has great possibilities, but he does not
know all the possibilities. He is the one who, in all probability,
deserves the greatest credit which will come from that invention,
and who should, I think, reap most of the benefits from it, but it is
frequently the case, and it is my belief, that there are men who
make a business of watching patents and studying the claims with-
out being any great inventors themselves, or without having any
great inventive genius, who study the claims of the patent and find
defects or omissions. In fact, those omissions may be things which
it is almost unnecessary to mention. Any man of intelligence would
consider that they are too obvious to mention, and he does not men-
tion them, but some man comes along and by mentioning these
same things gets a patent on them. He seeks even to get a patent
which would deprive a real inventor of carrying out his process, and
sometimes he succeeds in doing it. I do not know how that can be
righted. I believe that if a man has a process which is new, and
if he can prove that he had that process and was carrying it out
successfully before some one patented it, he should have the right
to it.

PROTECTION OF INTELLECTUAL PROPERTY 39

President Baekeland: The point of view developed so well
by Dr. Ittner is taken into consideration by the patent system of
the United States. Dr. Ittner is perfectly correct when he contends
that intellectual property should belong to the originator, whether
the latter desires to patent it or to keep it secret. However, this
country has devised the patent law as a way of making a "dicker"'
with the man who has a secret process. The nation says to him,
"If you will divulge your secret we will give you a monopoly for
seventeen years, but after that time, we confiscate your monopoly,
and then your invention shall belong to the public." This sounds
very well in theory, but in practice, the nation does not provide the
protection which was promised to the inventor, and the practice of
our patent system in the protection of patent rights is so difficult,
and leaves so many loopholes to the infringer, that the patentee in
return for the disclosure of his invention, practically gets a "gold
brick" from the nation, under the shape of a patent certificate,
which can only be enforced by wealthy people.

In theory, again, the American patent system provides for the
case explained by Dr. Ittner, where a process is kept secret for some
reason or another. For instance, it may happen that an inventor
does not possess the money to take out a patent, or much less to
defend his patent rights, if he had a patent ; therefore, he may think
it preferable to keep his process secret. By doing so^ he may run
the risk that his secret may be divulged. At any rate, he has a
good chance that instead of seventeen years' protection, he may
extend his monopoly for an indefinite time, not limited by law, and
only limited by the care with which he guards his secret. Or again,
a man may have invented a secret process, but may not think it
worth while patenting, or he may think no patent could be obtained
on it ; or, what happens frequently, he may have tried to obtain a
patent ; and have encountered an examiner who thinks he knows
everything and has decided that the subject matter is not patentable,
and who on this account may have rejected his claims. In the mean-
time another inventor, who has employed a more convincing patent
attorney, may have succeeded in obtaining a patent for practically
the same subject by formulating his claims somewhat dififerently. In
a case like this, the first inventor can, even after the patent of the
second inventor is published, file a new application and obtain an
interference. If he can prove beyond doubt that he is really the

40 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

original inventor, that he has pursued his work on this invention
diligently and continuously, that he has not merely taken up the sub-
ject at some time, then drop])ed it. then taken it up again after the
value thereof was demonstrated by the recent patentees; if, further-
more, he can prove that tlie subject matter has not been published
for more than two years, either as a patent or in some other publica-
tion, and if the process has not been worked commercially for more
than two years, he can still obtain a patent, which may in fact, be
entirely similar in wording and in claims to the patent of the other
patentee. Although the two patents may be coexisting, the only
valid patent will be the one for which, in interference proceedings,
priority of invention has been shown. All this sounds logical just
as far as the first inventor is concerned. Unfortunately, these inter-
ference proceedings are frequently very expensive to both litigants,
and may be complicated by appeals and reappeals and motions to
dissolve, and the patentee with the slender purse is again at a
tremendous disadvantage. In some cases, it is very difficult to fur-
nish evidence, and in more than one instance, interference proceed-
ings have been dragged out for many years and have cost the liti-
gants more than hundreds of thousands of dollars before the [)atent
was issued.

Other countries, for instance Germany, arrange this much
simpler. The only date of priority is the date of filing the patent,
as long as the invention is not known or published. This, of
course, puts a premium on the man who files first his patent. After
all, that is what the nation cares about: to have the benefit of an
early disclosure of the invention.

Furthermore, our interference system has another serious draw-
back. For instance, you may have obtained a patent in good faith
and feel entirely secure on account of it, and on the strength of your
patent, you have started an enterprise in which you put all your
own money, as well as the money of your friends. You go through
all the worry and difficulties and the risks of pioneership, and finally,
you succeed in convincing the world and the consuming public that
your invention is really a good thing, and just at the moment when
you are beginning to reap the reward of your enterprise, a man
steps in with an interference, which has been kept smoldering in
the Patent Office for several years. A new claimant arises, who
jumps at your throat and says, "Your patent or your business life,"

I

PROTECTION OF INTELLECTUAL PROPERTY 41

and drags you in endless and expensive interference litigation, where
the party provided with much cash and all that goes with it, is at
an overwhelming advantage.. If he succeeds in substantiating his
claim to priority, your patent will simply become invalid. This
gives opportunity for legally murdering a new enterprise. In fact,
the principle of our interference system is such that practically any-
body who starts any new industry, whether patented or not, and
which involves any process which is not so hopelessly old that it is
known all over the world, runs the risk that at any time somebody
may jump at him with an injunction on the strength of some long-
delayed patent application which has been "sleeping" in the Patent
Office. A striking instance of this has been given by the famous
Selden case, which involved the broad principles of automobile
construction.

In Germany, such absurdities cannot occur. The spirit of the
German patent law is very simple. It admits that the man who
discloses his invention by taking out a patent confers a benefit upon
the nation by becoming the teacher of the nation. Therefore, the
nation is willing to grant him patent protection for a certain number
of years. If, however, somebody has been carrying out the same
process secretly before the patentee filed his patent, the latter can
apply to the court, and if he can prove his case, the patentee may
be compelled to grant a free license for the personal' use of the
other inventor, who has first exercised this process in secret in his
own business. Indeed, in a case of the kind, the Germans reason
as follows: If a man already knew the process and was utilizing it
secretly in his business, but was not using it publicly before the
patent was filed, he received no benefit by the publication of that
patent. Therefore, he acquired the right of utilizing the process,
undisturbedly, at least for his own purposes in his own factory.
By keeping his process secret and by not filing a patent, he for-
feited, however, any claims to national protection under the shape
of exclusive patent rights.

Our American patent system may be very altruistic in concep-
tion, by the fact that it tends to reward the original inventor, whether
he discloses his invention or not, but the application of the system is
right away complicated with all the acrobatics of lawyers and all the
endless expense it involves. First of all, it is very difficult, in many
cases, to determine who is the first inventor.

42 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

The German system, not only has the merit of being incom-
parably simpler, but it rewards the inventor who confers a benefit
on the nation by disclosing promptly his invention. In this way, at
least, it is more beneficial to the nation at large.

Dr. Ittner also referred to the so-called "claim dodger." The
"claim dodger" is a dangerous animal in American patent law. He
is one of the worst modern, industrial pirates, although sometimes he
sails under the flag of a patentee. His existence in this country
is rendered possible by the tendency of Anglo-Saxon law to sacrifice
the spirit of any legal document to the letter of it. The German law
does not adhere slavishly to the mere wording of the claims of a
patent. It takes more in consideration the real substance of the
patent. The standpoint of the German patent law is summed up
as follows : What was the status of the art, what were the technical
efforts possible before the inventor filed his patent, and what
advance in the art has been rendered possible after the disclosures
contained in the patent ?

Just on this account, it is not necessary for a German to have
the absurd multiplication of claims which is the characteristic of
United States patents, and where quite often the mere cunning use
of the English language plays a greater role than the invention itself.

NOTES ON A STUDY OF THE TEMPERATURE
GRADIENTS OF SETTING PORTLAND CEMENT

By ALLEKTON S. CCSHMAN, The Institute of Industrial Research,
Washington, D. C.

Read at Joint Meeting with the Eighth International Congress of Af'f'tiea
Chemistry, New York City, September 4-13, 1912.

The reactions that take place when hydrauHc cements are tem-
pered with water and while the mixture is hardening are as yet not
understood. It is true that many theories have been advanced in
regard to the hardening process or processes, but more data is
required before much that now seems inexplicable can be understood.

Since all chemical reactions are accompanied by definite and
measurable thermal changes, complete temperature records of
hardening cements should yield interesting and valuable data.

It is well known that if a Portland cement clinker is ground
without the addition of from 2 to 3 per cent of calcic sulphate or
gypsum to act as a restrainer it will be "flashy." By "flashy" is meant
the tendency to harden very quickly, so quickly in fact that in many
cases it is impossible to mold the wetted cement into a plastic mass.
While this sudden hardening is going on, a considerable amount of
heat is generated so that the mass feels hot to the hand. The tem-
perature rises about 10° to 15° C, but the heat reaction lasts only
a short time and after cooling no further heat reaction takes place.
When, however, a Portland cement has been properly restrained
by grinding with it 2 or 3 per cent of g)'psum (plaster) the condi-
tions of thermal activity are changed in a quite extraordinary man-
ner. On mixing a normal Portland cement with sufficient water to
form a normally plastic mass, a certain amount of heat is imme-
diately disengaged, although not so much as in the case of an
unplastered cement. The plastic mass soon cools down to the air
temperature and generally falls somewhat below the surrounding
temperature, showing that a decided cooling effect is taking place.

43

44 AMERICAN IXSTITUTE OF CHEMICAL Ei\CIXEERS

If now the plastic mass is allowed to stand quiescent in a constant
temperature chamber, nothing of moment happens if the cement be a
normal standard brand, for a period of from four to eight hours.
At a given time, however, for every mixture a secondary heat rise
begins, and increases more or less rapidly to a definite maximum.
After this rise is completed the cement has attained its final set and
a gradual cooling takes place to the temperature of the surrounding
air and nothing further happens. If an imperfect, damaged or
lumpy cement is under observation the temperature gradient for the
rise may show aberrations. That is to say, a sudden rise may be
followed by a temporary cooling only to be followed by another rise.

The wonderful effect of a small percentage of g}'psum plaster in
thus controlling and regulating the temperature gradients or reaction
of setting cement is little understood and indeed presents certain
anomalous occurrences for our consideration, as will be shown
later on.

The first successful attempt to record the temperature gradient
of setting cement, as far as the writer has been able to ascertain, was
made by Gary, who used a photographic recording device, which has
been fully described by Burcartz.' The method consisted of placing
the bulb of an ordinary glass thermometer in the cement paste. The
whole arrangement was enclosed in a box through which a beam of
light was made to impinge through a slot, upon the graduated stem
of the thermometer and then upon a traveling photc^aphic film.
As the mercury rose or fell, the beam of light was cut by the
shadow of the mercury column and thus a continuous temperature
gradient record was obtained.

The only criticism of this method that can be made is that it calls
for an expensive and delicately adjusted piece of apparatus which
few laboratories would care to install, and in which the temperature
changes cannot be watched while they are taking place. The
apparatus used by the writer is simple, comparatively inexpensive,
and can be installed and used in any laboratory for making daily
records. The apparatus is shown in Fig. i.

A double walled wooden box, as shown in Fig. i. used simply to

avoid any sudden changes which may take place in the laboratory

temperature during a test run. An ordinary so-called "fireless

cooker," such as can be bought at any kitchen supply store, answers

1 Eng. Record, Dec. nth, 1909.

TEMPERATURE GRADIENTS OF SETTING PORTLAND CEMENT 45

very well for this purpose. The recording thermometer is of the
Tycos type and consists of a copper plated steel tapered mercury
filled bulb 9 cm. long by about 2 cm. in its maximum diameter.
The bulb is connected to the recording dial by a flexible steel
capillary tube. The recording dial has a range from 10° to 120° F.
The recorder is fairly accurate for the middle range and is easily
calibrated and adjusted.

In ordinary tests, as carried out in the writer's laboratory, i
kilogram of the neat cement is tempered with 250 cc. of water to
make a homogeneous plastic paste, which is packed into a No. 2

open-top tin can. The thermometer bulb is not inserted until the
primary heat effect which always develops when cement is kneaded
with water, is over, and the paste reaches approximately the same
temperature as the calorimeter box. In the meantime the copper
plated thermometer bulb is smeared with vaseline and wrapped with
several folds of fairly heavy tin foil. The object of these precau-
tions is two-fold : in part to guard against the "freezing" in of the
bulb when the cement hardens and in part to overcome any possible
pressure on the walls of the bulb if the cement shrinks or expands
during the hardening process. With 25 per cent of water the con-
sistency is somewhat softer than the normal, but experience has

46 AMERICAN IXSTirUTE Of CHEMICAL ENGINEERS

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TEMPER4TURE GRADIENTS OF SETTING PORTLAND CEMENT 47

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PLATE III.

TEMPERATURE GRADIENTS OF SETTING PORTLAND CEMENT 49

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50 AMERiay IXSTITVTE OF CHEMICAL ESCIXEERS

shown that the wetter mixture gives better results uniler the condi-
tions of the test. When all is ready the covered bulb is pushed into
the cement paste, care being taken that it is not pushed below the
surface so that the cement can close over the shoulder of the bulb
and so imprison it when hardening takes place. When these precau-
tions are taken the apparatus gives no trouble and the bulb is easily
withdrawn from the hard cement at the end of the test. The tem-
perature gradients are usually taken for a twenty-four-hour period,
although tliis is not necessary unless the full cooling curve is
desired.

In presenting these notes on the temperature gradients of set-
ting cements, it is not the intention of the writer to draw any
conclusions at this time in regard to the mechanism of the harden-
ing reactions.

The curves obtained on the revolving scale are transferred to
centigrade degrees and plotted in rectangular coordinates as is
shown in the illustrations, Plates I, II, III and I\', curves i to 32. An
inspection of the curves will show that in some cases the tempera-
ture gradients are much steeper and more sudden than in others.
Curves 6, 7, 8 and 21 represent cases in which the water was
simply poured on to the dry cement without previously kneading
the mass to a paste. In no case of this kind is a rise in tem-
perature noted following the final set or hardening, at about seven
to eight hours.

In the cases of some brands of cement, as is shown in curves
9, 10, II and 12, the rise in temperature is constant and gradual to
a maximum which usually occurs at about ten to eleven hours.
In other cases, notably in curves 17 and 29, the rise is sharp and
sudden. As both types of cement pass muster in the standard
tests, it is not possible at the present time to state what the ideal
temperature gradient curve for a cement should be.

That the maxima and shape of the curves is modified by the
addition of various salts to the tempering water, is shown in curves
13, 14, 15, 16, 17, 18, 19, 20 and 22.

Perhaps the most extraordinary curve is number 19, which shows
the heating effect produced by saturating the water with calcium
sulphate. In this case the temperature rose above the scale of
the recording device and the test piece became uncomfortably hot
to the hand. Since calcic sulphate is used as a restrainer when

TEMPERATURE GRADIENTS OF SETTING PORTLAND CEMENT 51

ground with a cement, this extraordinary effect of calcic sulphate
solution is difficult to explain.

Curves 25, 26, 27 and 28 were from cements which did not stand
test and had been rejected. The abnormality of these curves is at
once apparent to the eye and furnishes the best argument as to the
value of a study of the temperature gradient as an additional method
of control in cement testing.

In conclusion, the author wishes to point out that these notes on
the study of temperature gradients are offered not as data on which
to establish theories but to stimulate other workers to include simi-
lar investigations in their studies of the hardening of hydraulic
cements.

THE PRODUCTION OF AVAILABLE POTASH
FROM THE NATURAL SILICATES

«>■ ALLEKTOX S. CISHMAN and CEORGE W. CUGCESH ALL,
\Vu»hinf;toil, U. C.

Read at Joint Meeting with the Eiyhth International Congress of Apl<lied
Chemists. Sew York City. September 4-13, igi2.

The great demand which has recently arisen for an American
supply of potash in available form for agriculture, has stimulated
not only the search for new sources of this material, but also experi-
ments on a large and practical scale of operation, in the attempt
to develop a method of making the vast supply of potash locked up
in feldspars and feldspathic rocks either directly water soluble or
sufficiently soluble in dilute acids to insure a product which shall
be useful as a fertilizer. The natural silicates commercially available
as sources of potash are chiefly orthoclase and leucite. Both of these
minerals are potassium-aluminum silicates. The theoretical formula
for orthoclase is written KjO.AUOj.GSiO^. and for leucite
K20.Al,03.4SiO;. The principal sodium feldspar, albite, has the
theoretical formula : Na,O.Al,03.6SiOo. It is well known that these
feldspars run into and substitute each other in various proportions,
so that the products from different quarries will vary widely in
respect to their soda and potash contents. There is an enormous
supply of feldspar in the United States, both east and west,
which could be made economically possible as a source of potash,
provided the cost of production can be made low enough to compete
with the potash-holding manure salts which are at present so largely
imported from Germany. Although it must be admitted that the
imported potash salts are richer in potash than any product that can
ever be made from American feldspars, it should also be remembered
that the crude German manure salts contain large quantities of chlo-
ride and sulphates of elements which are not only undesirable in the
fertilizer but which may do actual harm under certain conditions.

52

AVAILABLE POTASH FROM THE NATURAL SILICATES 53

It is this fact which gives encouragement to the attempt to produce
from American feldspars a straight potash fertilizer which could be
used in exactly the same way that hardwood ashes have been found
useful.

Six general methods have been proposed for decomposing the
natural silicates in the effort to obtain water-soluble potash salts.

I. Adaptation of Natural Agencies. In the processes of Nature,
the slow action of moisture and atmospheric agencies, including the
action of carbonic acid gas, is known to have a decomposing or
kaolinizing action upon the feldspars. Immense deposits of feldspar
and granitic rocks have thus been decomposed, with the formation
of large beds of kaolin and clays from which the potash has been
leached into the surrounding valley. For this reason, the valleys
between feldspathic and granitic hills are usually highly productive
of the crops which require large amounts of potash, such as tobacco,
potatoes, large fruits, berries, etc. There have been a few processes
proposed, which depend principally upon the natural reactions has-
tened by pressure and other agencies. In 1904 Blackmore (U. S.
Patent 772,206) proposed the action of carbon dioxide gas under
five hundred pounds pressure upon a cream of the ground mineral,
repeated intermittently for several hours, in the attempt to produce
a yield of carbonate of potash. Ten years earlier the same experi-
menter (U. S. patent 513,001) had proposed using lime, calcium
chloride and steam pressure in an autoclave to produce chloride.
In 1910 Coates (U. S. patent 947.795) proposed the addition of
bacteria for the decomposition of feldspar. In 1910 Carpenter
(U. S. patent 959,841) proposed to heat the mineral intensely and
cool suddenly by plunging in water, in the effort to render the
feldspar amorphous, in the hope of making it more available for
plant growth. None of the above processes have as yet been shown
to possess industrial possibilities.

II. Wet Processes of a Chemical Nature. Levi in 1904 ( French
patent 344,246 and English patent 13,875) and Piva in 1905
(French patent 351,338) proposed methods for treating leucite by
means of solutions of alkali or alkali earth hydrates, generally under
increased pressure. The same general method for treating feldspar
was claimed by Swayze in 1907 (U. S. patent 862,676) and by Gibbs
in 1909 (U. S. patent 910,662).

Also Gibbs in 1904 (U. S. patent 772,612 and 772,657) proposed

54 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

a process of treatment with hycirofluosilicic acid, and subsequently
with sulphuric acid, in order to produce potassium snlpliate. In
1907 Cushman was granted U. S. patent 851,922, a public patent
which proposed a sludging of tinely ground feldspar with water, the
addition of a small amount of hydroHuoric acid and electrolyzing the
mixture in wooden cells provided with wooden diaphragms. Under
this process both potassium and aluminum hydrate passed through
the cell diaphragm into the cathode compartment. This process,
although perfectly practical, has not yet been made commercially pos-
sible owing to the high cost of hydrofluoric acid and the large amount
of by-products formed in the process. None of the above processes
have as yet been made commercial possibilities.

III. Dry Processes of a Chemical Nature, in which the Potash
Salts are Volatilized. In processes of this nature, fluxes, and in
some cases fuel, for producing purposes are ground and mixed with
the feldspar, the mixture being subsecjuently heated until the potash
salts are volatilized and collected either in the stack dust or par-
tially collected from the gases by passing them through or over
water. Swayze in 1905 (U. S. patent 789,074) heated ground feld-
spar with gypsum and carbon, and proposed to collect the volatilized
sulphate. Spencer and Eckel in 1909 (U. S. patent 912,266) made
a cement mixed with calcareous and silicious fluxes and green sand,
a natural potash-bearing iron silicate, clinkered the mixture in a
rotary cement furnace, and obtained a Portland cement, at the same
time collecting the potash in the stack dust and the flue gases. In
1911 Eckel (U. S. patent 1,011,172) proposed a somewhat similar
method, but heated only high enough to drive off the potash salts
and not high enough to clinker the mixture. Again in 191 1 Eckel
(U. S. patent 1,011,173) melted a mixture of green sand, lime-
stone and fuel, tapped off the melted iron and slag, and recovered
the potash salts from the flue gases.

Some of the processes under this heading have been tried on a
large scale. No great difficulty is recorded in driving off the potash
in the furnaces, but obstacles were encountered in the attempt to
collect the potash from the gases. As a by-product operation in the
manufacture of cements, these processes may yet come to be of
some industrial importance.

IV. Dry Processes which Propose to Separate Potash as
Hydroxide or Carbonate. The old method of Bickell, proposed in

AVAILABLE POTASH FROM THE XATURAL SILICATES 55

1856 (U. S. patent 16,111 ), whicli depended upon heating a mixture
of feldspar, lime, and natural phosphate rock or guano to a bright
red heat, has not as yet been proved practical or successful. The
process of the Soc. Romana Solfati in 1905 (French patent
352,275), which proposes the roasting of leucite with carbonate,
hydrate or nitrate of soda and lime and subsequently the passage of
steam through the roasted product to produce sodium aluminate
and potassium carbonate, is possible from a chemical standpoint,
but the high cost of operation has not nermitted the process to come
into commercial use. f

V. Dry Processes Producing the Chloride. These processes
have been most experimented with upon the mill scale of operation.

In 1900 Rhodin (U. S. patent 641,406) and in 1901 (J. Soc.
Chem. Indus, xx, 439) proposed fritting feldspar with lime and
salt. According to the published results, this experimenter obtained
good yields although theprocess has not become a commercial suc-
cess. In 1907 McKee (U. S. patent 869,011) suggested heating
a potash-bearing material containing mica with lime, salt and carbon
in order to obtain a yield of potassium chloride. Cushman in 191 1
(U. S. patent 987,436) proposed mixing feldspar with lime and
salts of a mineral acid capable of decomposing the silicate, giving the
mixture special treatment previous to heating in a rotary furnace in
order to produce the chloride. This method has been tried out on
a large mill scale of operation, and the results obtained will be
discussed later on in this paper.

VI. Dry Processes Producing Sulphates. In 191 1 Thompson
(U. S. patent 995,105) proposed heating to a bright red heat a

mixture of feldspar, sodium acid sulphate and sodium chloride,
and subsecjuently leaching out the potassium sulphate produced.
This experimenter claims that potassium chloride is first formed,
which is subsequently changed to the sulphate by the action of the
acid sulphate. It is stated that this process has recently been tried
on a commercial scale of operation. Sodium acid sulphate is a
by-product that is reasonably cheap, although a large quantity is
not available. The lack of an abundant supply of acid sulpWte is
perhaps the greatest drawback to the commercializing on a large
scale of this process, although it is possible that it may still become
of some industrial importance. Hart in 191 1 ( U. S. patent 997,671)
proposed to fuse feldspar with some barium compound, such as

56 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

tlie sulpliatc, together with carbon, to pulverize llie cool melt and
siibse(iuently to digest the i)roduct with sulphuric acid and thus
produce in solution potash alum and a residue of barium sulphate
and silica, which is claimed to be useful as a paint pigment. Hart
claims that some of the potash is volatilized during fusion. Sin'ce
the fusion temperature is 1500° C, it is probable that a considerable
])ortion of the potash does volatilize, and it is possible that this diffi-
culty may interfere with the commercial success of the process.

Wadman in 1907 (U. S. patent 847,856) proposed heating
lei)idolite with potassium sulphate and leaching the product with
sulphuric acid in order to obtain sulphates of lithium and potash.

A chronological list of the patents which have been granted for
the treatment of the silicates for the production of available potash
is given in Table I.

It would appear that the most promising processes for making
potash available from the natural silicates on a commercial scale
of operation are those wdiich are conducted in the dry way but
without actual fusion of the reacting mi.xture. Potash salts volatilize
readily at the high temperatures necessary for the fusion of the
silicates, and the collection of the volatilized potash from the stack
gases has not yet been carried out economically. A considerable
I)ortion of the potash does not settle in the dust chamber, and if
water sprays are used for washing the gases, the potash solutions
are very dilute and the cost of evaporation becomes prohibitive.
Furthermore, water sprays are found to interfere with the draft
regidation, even when the use of fans is resorted to. The mainte-
nance of artificial draft is an expensive and difficult matter, and is
very likely to interfere with the proper control of the furnace
temperatures. For work on the large scale of mill operation, a
continuous process must be used, avoiding fusion and with the regu-
lation of temperature to the exact point at which appreciable quanti-
ties of potash do not volatilize. The fluxes and reacting substances
must be cheap, available in large quantity, and the yields of water-
soluble potash salts must be high. The process which has seemed
to us to give the most promise of successful adaptation to commer-
cial ends is that of Cushman (U. S. patent 987.436) coupled with
tiie method of preparation of the materials before furnacing. pro-
posed and developed by Coggeshall (U. S. patent 987,554).

This process has recently been given extensive trials on a large

AVAILABLE POTASH FROM THE NATUR.IL SILICATES

57

Table I. — Proposed Extraction Processes Chronologically Arranged

Patentee

Year

Process

Product

IV

Bickell

1856

Lime, CaaCPOa, red heat

Caustic

I

Blackmore

1894

Lime, powdered CaCla, HaO,
steam

KCI

V

Rhodin

I goo

Lime, salt, heat under melting

KCI

11

Levi (leucite)

1904

Ca(0H)2 or NaOH, pressure
16 atmospheres

K silicate

II

Gibbs

1904

HoSiFe and HjSOj

K2SO4

I

Blackmore

1904

CO2 500 lb. pressure repeating

K2CO,

II

Piva

1905

(Leucite) KOH, NaOH,
steam 25 atmospheres

K silicate
K aluminate

IV

See. Romana Solfati

1905

(Leucite) alkali, carbon, CaO,
red heat

K2CO3

III

Swayze

1905

Gypsum and carbon, fuse, vol-
atilize

K2SO4

VI

Wadman

1907

Lepidolite, KaSO, H,S04 1 K2SO4

II

Cushman

1907

Water and HFl, electrolysis

KOH

II

Swayze

1907

Heat alone, then KOH sclu-
tion

K silicate
K aluminate

V

McKee

1907

"Containing mica" with CaO,
NaCl. and C

KCI

II

Gibbs

1909

Ca(0H)2, steam 150 lbs.

KOH

III

Spencer and Eckel

1909

Green sand cement mi.x vola-
tilize

K salts

I

Coates

igio

Bacterial action

I

Carpenter

1910

Intense heat, sudden cooling
alone

V

Cushman

1911

CaO, CaClz, etc., clumps, red
heat

KCI

VI

Thompson

1911

NaHSO,, NaCl, bright red

K2SO4

VI

Hart

1911

Ba compound as BaS04 and
C, fuse. H2SO4

Alum

III

Eckel

1911

Cement mix but not over 900°
C. with green sand volatilize

K2O

K2S04

III

Eckel

1911

Green sand, CaCO and C, melt
iron, volatilize

K2S04

scale and interesting results have been obtained. The process consists
essentially in powdering 100 parts of potash feldspar rock together
with about 20 parts of lime and with or without 10 to 20 parts
of rock salt. This powdered mixture is fed to the top of a
moving drum about three feet in diameter, in a layer about half an
inch deep. As soon as the layer is formed a strong solution of
calcium chloride is applied from a series of small tubes. The
CaCl, at once unites with the lime, forming a so-called oxy-chloride
cement, and a large portion of the mixed powder is thereby at once

58 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

fornifd into "clumps" or aggregates lying in a bed of surplus
powiier. As the drum revolves the bed is removed by a scraper to a
belt which delivers the mixture to a screen which separates th.e
clumps from the residual powder. The powder is returned by a
screw conveyor and elevator to the hopper above the drum again.
The clumps are about the size of peas and pass from the screen
directly to a rotary kiln similar to those used in burning Portland
cement. The kiln is heated by a blast of air and powdered coal in
the usual manner.

Th.e clumps pass regularly down through the increasingly heated
portions of the rotating kiln and roll out at the end, practically with-
out alteration in size and shape.

A large percentage of the total potash present in the feldspar is
converted into potassium chloride during the heat treatment, and
very little is volatilized. The dry clumps are of a pale yellow color
outside due to the iron in the ash of the bituminous coal used, but
they are snow white inside. The clumps are finally ground, pro-
ducing a pale yellow material containing as much water-soluble
KjO as hardwood ashes, although the potash is in the form of
chloride, and the product also contains considerable free lime.
Up to the present time no attempt has been made on a large scale
to leach out the soluble potash. The ground material is being given
field tests as a straight potash fertilizer containing lime.

A Resume of the Large Scale Experiments. Potash feldspars
were obtained from five different localities. Eleven carloads were
used in the trials, amounting to a total of 385 tons. Each carload
was ground and analyzed separately. The lowest in potash ran 6
per cent K„0 and 3 per cent Xa„0, the highest 11.3 per cent K^O
and 3.1 per cent Na„0. The bulk of the spar ran lo per cent
potash and 2 per cent soda, and the results given in this paper were
obtained on the 10 per cent spar.

The lime was a high calcium (|uick-hme. running about 90 per
cent CaO and 5.6 per cent Mgt).

The salt was rock salt from New York State and ran about 98
per cent NaCl.

The calcium chloride was obtained from the Solvay Process
Company. It was in the solid form and contained about 75 per
cent CaCl. and 25 per cent water.

All of the above materials are available in very large quantities

Feldspar

100

Lime

20

Salt

lO

AVAILABLE POTASH FROM THE NATURAL SILICATES 59

and at low cost. The calcium chloride is a by-product in the form
of a moderately strong solution, and but a small proportion is
concentrated au the present time, as the chief use is for refrigerating
purposes. Vast quantities are now run to waste. The solid form
was used in these trials merely for convenience.

Many heats were made with mipctures of varying proportions,
but the two mixtures used in the work here described were:

Feldspar lOO
Lime 20

Salt 20

The feldspar, lime and salt were separately crushed in gyratory
crushers and rolls, and dried in a rotary drier. In continuous work
the proper mixture would be made at this point by continuous
weighing machines, but as a number of different mixtures were to
be tried, each of the three raw materials was ground separately in
Huntington mills and put into bins. This preliminary grinding of
the feldspar and salt was to about 65 per cent through a lOO-mesh
sieve, of the lime about 83 per cent through the loo-mesh. The
weight per cubic foot of each powder of the above fineness was then
ascertained and measuring boxes were built so that the materials
could be separately measured out and run together into a large
mixing machine. Almost a ton w-as thus mixed each time. The
mixture was then conveyed to a tube-mill and further ground to a
fineness of from 97 per cent to 99.5 per cent through a loo-mesh
sieve, and then conveyed to the bin over the dumper and kiln.

The calcium chloride masses were broken up and thrown on a
perforted grid in a large tank holding about 48 tons. Water
was run in and the chloride dissolved most readily. The solution
was run out when about 42 degrees Beaume into two large
sump tanks and brought to a constant strength of about 42 per
cent CaCL. This was then pumped up to an elevated tank and
piped from there, through a constant level tank, to the dropper tubes
of the dumper placed in a row above the drum. This drum is 15.5
feet long and 3 feet in diameter, and is horizontal. There are 15
valved pipes, each one feeding an adjustable pipe holding 38 short
dropping tubes of brass 1-16 inch internal diameter, and set 5-16
inch apart.

60 AM ERICA X IXST/TUTE OF CnEMICAL ENGINEERS

The finely-ground mixed powder is taken from the bin by a
chute, elevator and screw conveyor and distributed in a long hopper
trough over the drum. It is taken from the trough by a roll device
and spread evenly on the moving drum at its topmost point. The
drum has a surface velocity of about 1.6 inches per second, the
layer of powder advancing at this rate.

It was found that by dropping the liquid very rajjidly upon the
powder, the clumps could be made rapidly enough to give a full feed
to the short rotary kiln when only one-third of the trough and drop-
pers and drum is used. A dumper drum 5 feet long produces every
hour almost two tons of fresh clumps and considerably over a ton
and a half of burned product with the kiln used in these trials. The
excess of powder passes through a screen and goes to the same ele-
vator which lifts the original material from the bin. The amount of
actual CaCL in the fresh lime is regulated to about 20 parts to each
100 parts of feldspar in the mixture. The clumps leave the screen
in rounded form and flow directly into the kiln.

The reason for the above procedure will now be explained. In
the first place, calcium cliloride reacts very efficiently under these
conditions with the feklsijar by replacing the potassium with cal-
cium, thus forming calcium silicate and potassium chloride.
Anhydrous calcium chloride is expensive to produce and it is im-
practicable to grind it into a mixture on a large scale on account of
the rapid absorption of moisture. Even if such a dry mixture
could easily be made, its use would present certain disadvantages.

When a reaction between an ore and solid fluxes is produced by
heating up to the fusing temperature, the reaction takes place on
the surface of the particles alone and only at the points where the
ore is in actual contact with the flux particles. Finer grinding will
produce a larger surface area and thus a greater number of actual
contact points, leading to a larger yield. There is, however, a degree
of fineness beyond which it is not wise to go, on account of the cost
of extremely fine grinding.

Another factor in the problem is brought out by the following
experiments : A batch of ore and the theoretical amount of solid
flux were ground together to just pass a 50-mesh sieve. This
powder, when subjected to a certain heat treatment, gave a reaction
yield of about 35 per cent of the theoretical. The mixture was then
ground to just pass a lOO-mesh sieve and given the same heat treat-

AVAILABLE POTASH FROM THE NATURAL SILICATES 61

ment. A reaction yield was obtained of about 65 per cent of the
theoretical. The mixture was then ground to pass a 200-inesh sieve
and again reheated as before. A smaller yield was obtained than
when the material just passed the lOO-mesh, although the particles
were undoubtedly only half the average diameter with about four
times the surface area, and should therefore have had far more
points of contact. Upon weighing equal volumes of the 50-mesh,
loo-mesh and 200-mesh powders, it was found that the latter con-
tained far less material and it became apparent that the 200-mesh
powder consisted for over 54 per cent of its volume simply of
voids. Such finely-ground powders are well known to "surge,"
that is, to show the tendency to flow like water through orifices in a
manner resembling fountains. Material ground as fine as this is
the cause of much trouble at spout slides and conveyors. Each
particle of a material of this extreme fineness is undoubtedly sur-
rounded by a film of air, the actual contact with the surfaces is
lessened and friction almost eliminated. When allowed to flow into
a bin, such a powder assumes an almost horizontal surface, there
is practically no angle of repose. Unquestionably the lessened con-
tact caused the low yields in the finely ground mixtures. Some of
the finer material was briquetted and the subsequent heat yield of
about 85 per cent of the theoretical. Briquetting is, however,
expensive and usually necessitates the addition of a binding agent
foreign to the reaction.

As a result of these investigations, the method was developed
for aggregating fine powders by dropping a suitable liquid upon an
excess of the powder in such a way as to cause a temporary bond
to form, thus practically eliminating the air films or voids around
the individual particles and permitting actual surface contact. Under
these conditions, with the same ore and flu.x used in the experiments
described above, the same heat treatment yielded within 3 per cent
of the theoretical quantity present. This method of aggregating
finely-powdered materials previous to furnacing has already been
used in several different ways. For example, in an ore mixture in
which the flu.xing material is an alkaline carbonate, such as sodium
or potassium, which forms crystalline salts containing water of
crystallization, if the carbonate is used in the partially anhydrous
condition and ground with the ore water alone dropped upon the
mix in the manner described formed at once a crystalline carbonate

62 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

wliich binds the particles of ore and flux into separate clumps, which
are hard enough to withstand screening, while the air films are prac-
tically eliminated. Using such a mixture and process as this, a
practically theoretical yield was obtained, altliough the flux was used
only in the exact molecular proportion called for by the reaction.

By this clumping process a very intimate contact of reaction of
surfaces is readily obtained at a low cost. The quantity of flux neces-
sary to complete the reaction is greatly reduced, the duration. and
temperature of the heat treatment is lessened, and working with
rotary kilns dusting and stack losses are almost entirely eliminated.
The clumps are beautifully adapted to the feed mechanism of rotary
kilns, as they flow easily, do not dust and take the heat more evenly
than fine powders. Now that the temperature conditions in rotary
kilns can be accurately controlled, it would seem that many chemical
and metallurgical reactions which are now performed by intermit-
tent processes and with low yields could be much more economically
carried out in continuous rotary kilns, taking advantage of this new
method of forming aggregates previous to furnacing.

In the application of this method to the treatment of feldspathic
rock, advantage was taken of the fact that a solution of calcium
chloride acts upon dehydrated lime to form the oxychloride, which
is a strong cementing compound. It was found that the formation
of calcium oxy-chloride gave a sufficiently strong bond to enable the
aggregates to withstand the operation of screening and the burden
in the kiln.

The theoretical quantity of calcium chloride flux required
depends upon the total quantity of K^O and Xa^O present in the mix,
as it is evident that the soda must also be liberated in proportion to
its content. The feldspar ore used ran lo per cent K,0 and 2 per
cent NaoO, which required theoretically 15.5 parts of calcic chloride.
In all our trials some slight excess of calcium chloride has been
used. The strength of the solution and the method of treatment has
been such that about 20 parts of actual calcium chloride are
present in the fresh clumps to every 100 parts of feldspar. The
20 parts of lime used is for the purpose of forming the aggre-
gates, and this lime remains practically unchanged in the finished
product. The presence of lime in a potash fertilizer will be found
advantageous to most soils, and it is generally admitted that lime
increases the manurial value of a fertilizer. If the object was to

AVAILABLE POTASH FROM THE NATURAL SILICATES 63

leach out the sohible potash sahs from the product, a much smaller
amount of lime could be used without interfering with the forma-
tion of hard clumps. The salt is added because it has been found
to aid the heat reaction, probably mechanically, as will be explained
later on. The fresh clumps contain from i6 to 20 per cent of
moisture, which is, of course, evaporated in the upper part of the
kiln.

The rotary kiln used in these trials was one of the old bottle-
shape cement kilns with a total length of slightly over fifty-five
feet, the upper twenty feet having a diameter of four feet clear
inside the firebrick lining, the lower portion widening out to nearly
six feet inside diameter. The pitch was seven-eights of an inch per
foot, and the most suitable speed was found to be one revolution in
about two and one-half minutes.

The conditions of the heat treatment are very important. The
kiln used was too short to yield the best results, and after the pre-
liminary experiments changes were made which caused the material
to take about one and one-half hours to pass through the length of
the kiln. The temperature of the gases issuing from the upper end
of the kiln were read continually with a thermo-couple pyrometer
fitted with a 15- foot fire end and temperatures were also taken
from time to time at the liring platform. A furnace wall tem-
perature of about 1370° C. is required for efficient burning of
powdered bituminous coal. This is, however, much too high a tem-
perature for potash work in a rotary kiln. This difficulty called for
careful experimental investigations and adjustments of the heat
treatment before the proper yields could be obtained. If a longer
kiln had been available, there is every reason to believe that a more
efficient use of the heat could have been obtained. The coal used
was a fairly high volatile bituminous coal. It was ground to
about 94 per cent through a lOO-mesh sieve and blown into the
furnace under an air piressure of about ten pounds per square
inch.

During the progress of the clumps down the kiln the following
reactions probably take place. At the entrance to the kiln the water
begins to evaporate. As the hotter zone is approached, the tem-
perature rises high enough to melt calcium chloride and salt.
Whether the calcium chloride is free to melt is not known to us, as
the exact composition of the oxy-chloride compound formed has not

6i AMERICAN INSTITUTE 01- CHEMICAL ENGINEERS

yet been determined. The results of our work seem to prove that
the reacting chlorine is more readily evolved from the oxy-chloride
compound than it is from calcium chloride alone. The melting of
the salt, however, continues the bond of the reacting particles, caus-
ing them to thoroughly "wet" each other, and from this point on
the attack on the silicate proceeds rapidly. During the heating
usually from i to 2 per cent of NajO is volatilized.

When operating with no salt present, the yield of soluble potas-
sium chloride was 47.5 per cent of that originally present in the
feldspar. On adding to the mixture 10 parts of salt to each 100
of spar, a test heat yielded 64 per cent, but of this 9 per cent was lost
by volatilization, giving a yield of 55 per cent net in the final
product. On adding 20 parts of salt to the mixture, the yield grows
to 69.2 per cent with no volatilization, and to 75 per cent under
heat conditions which caused a volatilization of 7 per cent, leaving
a net yield of 68 per cent of that originally present. In the case of
clumps made from a mixture of i(X) parts of feldspar containing 10
per cent K^O and 2 per cent NajO, 20 parts of lime, 20 parts of
salt and 20 parts of calcium chloride, the theoretical composition if
no volatilization loss takes place, is shown compared with the actual
results obtained in the following table :

Theory Analysis

Total K2O 6.2S% 5-8%

Water soluble K2O 42 Equals 6.65% KCl

Loss of KjO .... 0.5 As KCl already formed

Total Na;() 7.62 7.1 52% made into NaCl

Water soluble NaiO 6.37 5,1 Showing 1.79% vaporized as

NaCl or 26% of that present.

This particular product contained 11.2 per cent of free lime
and total lime by analysis 15.5 per cent. There was also in this
sample about 5 per cent of free unchanged calcic chloride. The
amount of calcic chloride in the various runs made up to the present
time have been reduced gradually to about i per cent, and it is felt
that in the future better conditions of heat treatment will make coin-
plete use of the calcic chloride and at the same time raise the yields
of soluble potash. In later runs in which only 10 parts of salt were
present in the mix, the theoretical and actual analysis of the product
was as follows :

AVAILABLE POTASH FROM THE NATURAL SILICATES 65

Theory Analysis

Total K2O 6.66% 5.62%

Water soluble K2O 4.5 Equals 7. 1 2^0 KCl

Vaporization loss of soluble K2O 1.04 As KCl already formed

K2O insoluble in water 1.12

Total Na20 41S

Water soluble NajO 3.7 Showing 0.45% vaporized as

NaCl or 11% of that present.

This product contained 12.25 per cent of free lime, the total
potash rendered soluble was 5.54 per cent of the product or 83.2 per
qent of the total quantity present, but as 15.6 per cent had been
volatilized the net yield in the product amounted to 67.6 per cent.

The material which was later made continuously according to the
process described above carries 4.5 per cent of water soluble KnO
in the form of 7.12 per cent potassium chloride, and in addition to
this material carries only 1.12 per cent K^O insoluble in water. It is
well known that a 2 per cent citric acid solution will extract, when
used according to the Wagner method somewhat more KjO than can
be made directly water-soluble. This fact is of considerable interest
when the product is to be used directly as a potash fertilizer.

Conclusion. It is believed that under better conditions of heat
treatment which can be obtained with longer kilns and with a some-
what different arrangement of the combustion chamber slightly
better yields than those reported can be obtained. It should be
remembered that the kiln used in these experimental trials was
originally designed for burning cement, but this type of kiln has
long been superseded by improved forms. In order to get the proper
heat treatment in the middle of the kiln to complete the reaction, it
was necessary to have the upper part too hot. This condition will
not maintain in a properly designed kiln. It is also believed that the
use of oil as fuel would have allowed an easier regulation of the
heat treatment, but the trials so far undertaken have been made
under conditions which were found available at the time.

The subject of the costs of this process and of the product can-
not be gone into in detail at this time, but a few general statements
may be made. The production of water-soltible potash in feldspathic
rock is essentially a low-grade proposition, and the commercial
success of such a process depends upon the low cost of the various
operations. The manufacture of a straight potash fertilizer con-
taining as valuable ingredients only potash and lime must be carried

66 AMERICAN ISSTITVTE OF CHEMICAL ENGINEERS

out on a very large scale and by the most niotlern methods of con-
tinuous operation. With regard to the clumping process, the trials
have shown that this operation can be practically carried out as a
continuous process and at an exceedingly low charge per ton of
product.

The process may be directly compared with that cf the manu-
facture of Portland cement. It is a little easier to grind feldspar and
lime than the shales and limestones used in cement manufacture.
Drying will cost no more. Chemical control of the raw mi.xes will
not be more expensive and perhaps much less. Clumping, as has been
shown, adds a very small charge to the expense of treatment. The
cost of furnacing the feldspar mix will be less than similar charges
in the cement industry, as the temperatures required are much
lower and less coal is consumed. The product from the potash kiln
is comparatively soft and pulverizes easily in hammer mills, while
the charges on the cement industry for grinding clinker is an
important item. Again the softer product merely requires to be
ground fine enough for use as a fertilizer, whereas cement clinker
must be ground very fine and costs rise rapidly with increasing
fineness. Repair bills in the case of feldspar treatment should be
much smaller than in cement manufacture. The charge for raw
materials is somewhat larger than in the case of cement, but this
is more than met by the smaller costs of operation.

The potash fertilizer as now produced should be equal in fertil-
izing value to the ordinary grades of hardwood ashes. The product
carries practically the same content of water-soluble potash and
somewhat more lime than wood ashes. There is every reason to
believe that if the process becomes an industry the yields of
water-soluble potash can be considerably improved. The material
yielded is not a fused product, it is friable as an ash and it has the
physical texture to make it a valuable aid to soil structure. The
success of the product must, of course, depend upon the results
obtained under test conditions in its experimental use as a fertilizer.
If results are obtained which are as good or better than those which
usually attend the proper use of high-grade wood ashes, it is believed
that there should be no reason why this product cannot be success-
fully produced and introduced, especially in those parts of the
country where potash feldspars, fuel and shipping facilities are
available.

AVAILABLE POTASH FROM THE XATCR.IL SILICATES 67

Summary. In this paper a summary is given of the various
processes which have been proposed for making the potash in the
natural silicates available as a fertilizer.

Experimental trials of a new rotary kiln process for treating
feldspar are described, which depends upon a previous treatment
before furnacing, consisting of a method of aggregating or clumping
the mix so that chemical contact of the reacting substances is
brought about during the subsequent processing. The qualitative
and quantitative results obtained on a number of experimental trials
on a mill scale of operation are presented and discussed. It is
shown that it is possible to economically manufacture a potash fer-
tilizer containing free lime from feldspar and for a sufficiently low
cost to make an industry based upon the method, worthy of
consideration.

POTASH, SILICA AND ALUMINA FROM FELDSPAR

Uy EDIVAKD IIART

Read at Joint Meeting with the Eighth I nternational Congress of Applied
Chemistry, New York City, September 4-13, 1912.

In a study of the commercial utilization of feldspar which 1
undertook several years ago, it soon became evident that the potash
alone would not pay the cost of extraction. This is the cause of the
commercial failure of all the methods heretofore proposed. It is
necessary, therefore, to separate and put into marketable form the
other constitutents — silica and alumina — if our method is to be
successful.

With this purpose in view I have finally worked out the follow-
ing process which gives good prcspect of commercial success :

The feldspar chosen should contain not much less than 12 per
cent potash. Spar of this quality can be obtained in quantity, but
one of the pitfalls inventors must avoid is the expectation of getting
spar containing the theoretical 16.9 per cent of potash. The spar
mixed with the proper amount of potassium sulphate and carbon is
fused. The carbon added is so regulated that the resulting slag
contains a considerable proportion of sulphides. This has the double
advantage of saving a part of the sulphur, disengaged as hydrogen
sulphide on dissolving in acids, which aids also in the complete
decomposition by breaking apart the particles as it is given off.
Experiments show that if a colorless slag is obtained of even higher
alkali content it is much less easily decomposed by sulphuric acid.

The slag so obtained must be very finely pulverized and treated
in closed vessels with dilute sulphuric acid leaving behind a very pure
silica which needs only washing and ignition to yield a marketable
product fitted for the potter's use or for the manufacture of sodium
silicate.

The solution contains potash alum and any small amounts of
other metals such as iron, manganese and soda as sulphates. Lime
is inadmissible, as the sulphate forms crusts on evaporating.

POTASH, SILICA AND ALUMINA FROM FELDSPAR 69

The solution on cooling g^ves at once crystals of alum, which,
washing with a little water and centrifuging. renders marketable.
Any iron present remains as ferrous sulphate in the mother liquor.
Alum, however, is marketable only in limited quantity and must
be, for the most part, converted into its constituents, aluminum and
potassium sulphates. This is easily done by adding to the solution
in a closed vessel potassium sulphide in slight excess when aluminum
hydroxide mixed with a little sulphur precipitates in a form easily
washed. This is dissolved in hot sulphuric acid, run through a filter
and allowed to solidify. The potassium sulphate is obtained by
evaporation.

Each ton of feldspar (12 per cent K„0 ) should yield 444 lbs.
KjSO,, 2040 lbs. commercial aluminum sulphate ( 18 per cent
AI2O3), and 1300 lbs. SiOo.

Gayley Chemical and Metallurgical Laboratory,

Lafayette College,

Easton, Pa.

A CHEMICAL INVESTIGATION OF ASIATIC RICE

ISy ALI.KKTON S. C'lISHMAN and II. C. FCLLKR, Institute of IniluHtrtal
Ueseui'Cli, AVasliingtuii, D. C.

Read at Joint Meeting zvith the Eiglit International Congress of Applied
Chemistry, New York City, September 4-13, 1912.

Introduction. — The following paper contains a description
and the results of a complete chemical investigation of twenty-
seven samples of Asiatic rice, which was recently carried out at the
instance of the Siamese Government. The samples were collected
in the open makct at Singapore and Shanghai and no effort was
made to prepare them in any way differently from those rices which
are ordinarily exposed for sale in the Asiatic market. The relation
of an exclusive rice diet to the etiology of beri-beri disease has been
much discussed for a number of years past. This paper does not
pretend to decide this controversy but is offered as a contribution
to the general knowledge of the chemical constitution of rice. As
far as the authors are aware the results on the phosphate content of
eastern rices is the most complete yet published.

Description of Samples. — The samples reached the Institute
on October 30th, 191 1, and the box containing them was opened on
October 31st. The samples were contained in twenty-seven 10
pound cotton bags numbered serially i to 27. No other distinguish-
ing marks or information was found.

The cotton bags were found to be frail and rotten and in some
cases were broken through, so that the contents had partially
escaped. All the samples contained living weevils, and a few worms
and beetles were also found. The condition of the samples made it
necessary to hand pick them to remove insects. Th'ey were then
immediately packed in glass bottles, stoppered and labeled.

The appearance of the samples indicated that they represented
a medium grade of white or milled rices. On the trip from the
Far East the samples had evidently suffered desiccation with the

70

A CHEMICAL INVESTIGATION OF ASIATIC RICE 71

result that some of the grains had become abraded and broken.
As it was not believed, however, that the grain had suffered in
such a way as to affect the chemical analysis except in regard
to moisture content and the weight per lOO grains, it was decided
to be unnecessary to delay the investigation by awaiting a new
importation of samples from the Far East.

The Analytical Work. — The analytical work was carried out
by the methods recommended by the Association of Official Agricul-
tural Chemists of the United States, and comprised the following
elements usually sought : Moisture, Ash, Proteids, Ether Extract
(mainly Fat), Fibre, Starch and other Carbohydrates, Weight per
loo Grains.

The above determinations have usually been accounted sufficient
to fix the nutrition value of a given cereal. In view, however, of a
recently published claim that milled rices are deficient in organically
combined phosphorous, phosphate determinations were carried out
on each sample. The results have been carefully checked and may
be taken as accurate for the samples worked on.

Tabul.\tion of Results. — The results of the analytical work
on the twenty-seven samples submitted are given in Table I, with
the exception of the phosphate contents which are tabulated
separately in Table III. Table II gives the results of analysis of
two fresh samples of South Carolina (U. S. A.) rices bought at a
prominent grocery house in Washington, D. C. These samples are
denominated Numbers 29 and 30. Sample 29 is the ordinary very
white large grained rice as sold in the United States at about ten
cents a pound. Sample 30 was sold for a slightly higher price and
purported to be a "natural uncoated special pure rice." Table III
gives the phosphate content of all samples, reported as phosphoric
anhydride, P2O5. In Appendix A are given the results of an
examination of various rices exhibited at the World's Columbian
Exhibition, at Chicago, in 1893, the analyses made by the Division
of Chemistry, U. S. Department of Agriculture. Appendix A is
preceded by an extract from Bulletin No. 13, and is followed by a
summing up of the results.

72

AMERICAN INSTITUTE OF CUEMICAL ENGINEERS

TABLE I

Results of Analysis of Twenty-seven Samples of Rice Submitted to the

Institute of Intjustrjal Research by the Siajiese Legation,

Wasuincton, D. C.

Sam- ^
S'o. "

height of
0 Grains.

Moisture.

Ash.

Ether
Extract.

Crude
Fiber.

Proteids.

Starch
and Carbo-
hydrates.

I I

565 gms.

lI.02Cc

0.46%

0.31%

0.40%

8.13%

79.68%

2 I

539 "

10. 99

0.51

0.29

0.60

8

25

79 36

3 I

181 "

II. II

0.56

0.20

0.29

7

38

80.46

4 I

036 "

10.82

0.46

0.15

0.20

8

44

79 93

S 1

708 "

11-54

0.40

0.13

0.82

8

44

78.67

6 I

651 "

10.51

0.49

0.28

0.83

S6

80.33

7 I

498 "

II. 14

0.50

0.20

0.72

81

79 63

8 I

244 "

11.31

0.48

0 15

0.47

75

79 84

9 I

481 "

11.10

O.S5

0.68

0.66

31

78.70

lO I

409 "

11.3°

0.41

0 63

0.43

81

79 42

II I

3-9 "

10.60

0.49

0. 20

0.21

63

80.87

12 I

725

11.28

0.47

0 31

0.27

56

80.11

'3 I

723 "

10.45

0.45

0.17

0.60

06

80.23

14 I

541 "

10.94

0.44

0.53

0.76

56

79-77

IS I

141 "

10.44

0.54

O.IO

0.31

81

80.80

i6

11 .08

0.8s
0.74

0.28

0.44
0.16

8

25

81

79.10
80.66

17 o

958 "

10. SI

0.12

7

i8 o

892 "

10.49

0.60

0.30

0.32

8

00

80.29

10 o

788 "

9 99

0.48

0.94

033

8

06

80.20

20

10.06

055

1-23

0.71
0.80

0 51
0.77

8

«3

44

80.04
79 55

21 I

238 "

9.21

8

22 I

175 "

9.19

0.72

0.87

0.56

8

94

79 72

23 I

533 "

932

0.57

0.52

0.45

8

75

80.39

24 I

179 "

9 55

0.77

0.91

0.47

8

38

79.92

25 1

429 "

10.37

0.58

0.16

0.23

8

38

80.28

26 I

413 "

10.04

0.72

059

0.45

7

63

80.57

27 I

581 "

10.81

0-5I

0.44

0 31

8

■63

79 30

TABLE II
Result of Analysis of Two Samples of South Cakolina Rice

Sam-

Weight of
100 Grains.

Moisture.

Ash.

Ether
Extract.

Crude
Fibre.

Proteids.

Starch
and Carbo-
hydrates.

29

30

2 . 241 gms.

2.238"

10.23%
9.01

0.47%
0.37

0.42%
0. 21

0.29%
0.36

9-00%
8.13

79 59%
81.02

A CHEMICAL INVESTIGATION OF ASIATIC RICE

73

TABLE III

Results of Phosphate Determinations on Twenty-seven Samples of Rice

Submitted to the Institute of Industrial Research by the Siamese

Legation, Washington, D. C.

Soulh Carolina rice.

Sample No.

Per Cent PjOs.

Sample No.

Per Cent PiOs.

Sample No.

Per Cent P20s'

I

O. 22

10

0-3I

19

0-3I

2

o 39

II

0

32

20

0

30

3

0.30

12

0

23

21

0

41

4

0. 20

13

0

21

22

0

39

5

0.28

14

0

21

23

0

42

6

0. 26

15

0

30

24

0

58

7

0.31

16

0

49

25

0

24

8

0. 26

17

0

35

26

0

22

9

0.30

18

0

35

27

0

34

Interpretation of Results. — A careful inspection of the
results shows, that all of the analyses of the samples submitted
compare favorably in respect to nutrition value with the samples
given under the World's Fair report which includes typical rice
analyses as quoted by various authorities (see Appendix: A). The
results also for the most part compare well with the analyses of the
South Carolina rices given in Table II. The phosphorous content
of the imported samples (Table III) shows considerable variation;
in some cases it corresponds to the average for milled white rice
which is reported to be about 0.25% ; in other cases it is as high as
is usually shown in rices treated by the parboiling process. It
would appear that the white rices as represented in the twenty-
seven imported samples show on the average as high a nutrition
value as the white rices from other sources. The moisture content
and weight per 100 grains is somewhat low in the imported samples,
for the reason stated above.

Interpretation of the Analytical Results in Relation to
the Etiology of Beri-Beri. — It has recently been claimed by
Doctors Fraser and Stanton of the Institute for Medical Research,
Kuala Lumpor, that the low phosphorous content of white milled
rices is a predisposing cause of beri-beri. (See "The Lancet,"

74 AMERICAN L\ST/TUTE OF CHEMICAL E\CI.\EERS

London. \'ol. 176, p. 451. 1909.) It is further stated by Doctors
Fraser and Stanton tliat: "From epidemilogical conditions and
from experimental evidence it appears that Siam rice is considerably
more potent in its beri-beri producing powers than Rangoon
rice."

Opposed to the conclusions of Doctors Fraser and Stanton stands
the opinion of Dr. Hamilton Wright, former Director of the Insti-
tute for Medical Research, Federated Malay States, an eminent
investigator of the Etiolog)' and Pathology of Beri-beri. Dr.
Wright's published opinion,* based on years of study and clinical
experimentation is quoted below :

"The theory of the causation of beri-beri that fits the above
facts and all others observed in British Maylaya is that beri-beri
is due to a specific organism which gains entrance to the body
via the mouth, that it develops and produces a toxin chiefly in the
pyloric end of the stomach and duodenum, and that the toxin,
being absorbed, acts atrophically on the peripheral terminations of
the afferent and efiferent neurones. Further, that the specific
organism escapes in the faeces and lodges in confined places through
accident or the careless personal habits of those affected by the
disorder, and that in the presence of congenial meteorological,
climatic and artificial conditions of close association from over-
crowding, the organism becomes virulent and, gaining entrance to
the healthy body in food, etc., contaminated by it. gives rise to an
attack of the disease. The fact that the germ remains so closely
focal can, I think, be explained by its being at once destroyed by
the action of direct sunlight or that the presence of CO; or some
other gas is necessary for its virile development. It seems from
my observations here that the active stage of the organism in the
body is between three and four weeks. I base this estimation on
the facts that the preliminary feeling of oppression in the epigas-
trium ceases at the end of about three weeks, and that it is rare to
find the lesion of the pastric and intestinal mucose in cases of only-
six weeks' standing."

Conclusion. — As far as the results of analysis can be inter-
preted in the light of the information at hand, there would appear

* An inquirj' into the Etiologj- and Pathologj- of Beri-beri. Hamilton
Wright, M. D., Studies from Institute for Medical Research, Federated
Malay States, Vol. 2. N'o. i. p. 58 (363).

A CHEMICAL INVESTIGATION OF ASIATIC RICE 75

to be no reason wliy the white milled rices from one section of the
world should be held more responsible for mal-nutrition than
similar rices from other sections.

APPENDIX A.

Extract from Bulletin No. 13,* U. S. Department of Agri-
culture, Division of Chemistry.

Rice may reach the analyst in three different states, viz. :
unhulled, hulled, and polished. He may also have occasion to
examine the broken fragments used in polishing and hulling, the
waste in manufacturing rice bran and other products. The most
important of these products in the present connection is the
polished rice as it is found in commerce, ready for preparation
as food. Rice is a cereal in which the starchy matters predominate,
and in which there is a marked deficiency of proteids and oils as
compared with other standard cereals. The composition of rice,
as determined by the analysis of samples exhibited at the World's
Columbian Exposition, and by standard authorities, is best shown
in the table of maxima, minima, and means, as in the case of the
other cereals which have been mentioned. In the following table
the items marked I, II, and III, represent data obtained at the
World's Columbian Exposition, while the means of all the samples
there analyzed are given in another part of the table.

The mean composition of the different classes of rice as shown
by the analyses of the World's Fair samples is almost the same
as that shown by the work of other analysts collated as indicated
above. A typical unhulled rice has about the following composi-
tion:

Weight of 100 kernels, grams 3 .00 Crude fibre, per cent g . 00

Moisture, per cent 10.50 Ash, per cent 4.00

Proteids, per cent 7 ■ 50 Carbohydrates, other than crude

Ether extract, per cent i . 60 fibre, per cent 67 . 40

♦Foods and Food Adulterants. Investigations made under direction of

H. W. Wiley, Chief Chemist, Part 9. Cereals and Cereal Products, Wash-
ington, D. C, 1898.

76 AMERICAN INSTITUTE OP CHEMICAL ENGINEERS

Table of Maxima, Minima, and Means of Constituents of Rice

Kinds'and Numbers of
Samples.

Weight
of loo
Kernels.

Ash.

Carbo-
h yd rales,
Exclud-

1. Rice in the hull (for

eign) :

Maxima

Minima

Means

2. Unpolished rice (for-

eign) ;

Maxima

Minima

Means

3. Polished rice (foreign) :

Maxima

Minima

Means

Mean composition of pol
ished rice, etc., as
given by Jenkins
and Winton.

Polished rice (10 anal
yses)

Rice bran (5 analyses)

Rice hulls (3 analyses)

Rice polished (4 anal-
yses)

Mean composition of rice
etc., as given by
Konig.

UnhuUed rice (3 anal-
yses)

Hulled rice (41 analy
ses)

Polished rice (9 analy-
ses)

Means of World Fair
samples.

Unhulled rice (4 anal-
yses)

Unpolished rice (6
analyses)

Polished rice (14 anal-
yses)

3-250

2.842!

2.979

.826t
.260I
.466

-633t
.S6o*
•132

2 929
2.466

2.132'

11.52!
9 03
9.88

i2.S7t
10.92!

13.1st
II.82t

12-34

12.40
9.70
8.20

11.99
12.58

12.52

8.4ot
8.23"'
8.32

10. sot
7.27t
8.02

iO-33t

S-42t

7-18

7.40

12.10
3-60

10.00 I 11.70

7-52

7 95
8.02
7 18

2.04t

I 44
I. 71

2.26t
1.62^

1.96

o s4

0.04t

0.26

0.40
10.90
0.70

6.48 1. 6s
6.73

0.84

1. 6s
1 .96
o 26

ii.47t
9.45t
10.62

i.ooj
o.87t
093

0.56'
0.27'
0.40

0.20
9-5°
35-70

6.30

6.48
1-53
0.48

10.42
o 93
0.40

4.66*
3 -261
4.12

I.22t
l.04i
I IS

0.6s*

0.28

0.46

0.40
10.00
13.20

6.70

iii
0.82
0.64

4.09
i-iS
0.46

' Guatemala.

t Johore.

X Japan.

A CHEMICAL INVESTIGATION OF ASIATIC RICE 77

A typical hulled rice, but unpolished, has about the following
compositions :

Weight of loo kernels, grams .... 2 . 50 Crude fibre, per cent i . 00

Moisture, per cent 1 2 . 00 Ash, per cent i 00

Proteids, per cent S . 00 Carbohydrates, other than crude

Ether extract, per cent 2.00 fibre, per cent 76.00

A typical polished rice has a composition represented by the
following numbers :

Weight of 100 kernels, grams .... 2 . 20 Crude fibre, per cent o . 40

Moisture, per cent 12.40 Ash, per cent c.50

Proteids, per cent 7 . 50 Carbohydrates, other than crude

Ether extract, per cent 0.40 fibre, per cent 78.80

THE BEEHIVE COKE OVEN INDUSTRY OF THE
UNITED STATES

By A. W. BEUDEN,' Bureau of Mine* Experiment Station, Pittsburgh, Pa.

Read at Joint Meeting with the Eighth International Congress of Afplied
Chemists, New York, September 4-13, 1912

The manufacture of coke in the United States according to
authenticated reports was begun about 1817. From this date on,
mention is made from time to time of the use of coke for metal-
lurgical purposes, but the coke was made on the ground in pits
or mounds and no record of any coke made in ovens can be found
until the year of 1841 when two carpenters and a stone mason
formed a partnership for the building of two ovens and the
manufacture and sale of coke. This plant was built in the famous
Connellsville region, and although the business venture was
unsuccessful the coke proved useful for foundry purposes. This
venture, together with experiments carried on during the ne.xt
ten or fifteen years, fully demonstrated the value of this fuel, and
production increased by leaps and bounds into the vast beehive
coke oven industry which completely dominated the field until
1893, when the first coke oven plant for the recovery of by-products
was introduced into this country.

The evolution of the modern beehive oven started as shown
above and the process of coking in this type of oven has not
materially changed, the modern increased efficiency being due in
great measure to improvements in the ovens and the preparation
of the coal before charging into the ovens.

BEEHIVE OVE.NS

The beehive oven in its essential details may be described as a
circular vaulted fire-brick chamber constructed on a suitable
foundation, with flat tile bottom, an opening in the top through
* Published by permission of the Director of the U. S. Bureau of Mines.

BEEHfVE COKE OVEN INDUSTRY OF THE UNITED STATES 79

80 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

which the coal is charged and the products of combustion escape,
and an arched door at the bottom about three feet high, through
which the air for combustion is admitted and the coke watered
and drawn. Tiie many variations and improvements since the
ten-foot-diamcter oven of the carpenters and stone mason of 1841
have led to the present standard beehive oven as shown in section
Figure i. The size of the door and the trunnel-head. height of
dome and diameter of oven vary in different localities, but the
essential features are the same. The ovens are built in single
rows called bank ovens or in double rows back to back or stag-
gered. The coal, the amount of which is previously determined
as the oven is to be burned 48, 72 or 96 hours, is charged into the
oven from a larry car operated on a track above the ovens. The
coal in falling into the oven forms a conical pile and is leveled by
means of a scraper operated by hand. The door is bricked up to
within two or three inches of the top and the oven left until the
heat held by the bricks from preliminary heating, or the previous
charge, raises the temperature to the point where the volatile
matter, distilled from the coal, finally catches fire. The coking
proceeds from the top downwards and the burning of the volatile
to maintain the recjuired heat is regulated by closing up the air
opening as the amount of the volatile falls off. After the volatile
has ceased to come off the process is finished. The door is then
torn down, the coke watered on the inside of the oven by means of
a spray of water and is then drawn from the oven.

The beehive oven arranged for the mechanical drawing of coke
differs from the above only in the width of the door and project-
ing iron jams at the sides of the door. Mechanical drawing of the
beehive oven has been resorted to on account of tlie scarcity of
labor and not from any increased efficiency resulting from the
mechanical operation per sc. There is reason to doubt if
mechanical drawing shows any material reduction in the cost of
operation when all the items are taken into consideration. It
unaoubtedly breaks up the coke more, producing a large percent-
age of breeze, but, on the other hand, it reduces the time of draw-
ing very materially. The enlarged size of the door makes
draftmg more aifficult and leads to much burned coke. The
practice of watering far in advance of drawing and especially
where the precaution of putting the lid on trunnel-head is not

BEEHIVE COKE OVEX IiXDUSTRY OF THE UNITED STATES 81

followed, leads to the rapid cooling of the oven and reduces the
yield by increasing the length of time necessary for subsequent
charges to ignite. This increases the time to burn the same size
of charge or necessitates the reduction of the charge to burn ovens
down on time.

Lately a patented machine for the mechanical leveling of coal

in beehive ovens has been put on the market and is now in opera-
tion in the Connellsville coke region (Figure 2). It runs on the
larry track, uses the larry trolley, and operates through the trun-
nel-head. This machine gives evidence of proving its visefulness,
not orUy by the elimination of hand labor, but by encouraging
the proper leveling of the ovens, an operation too often neglected
or considered of little importance. The proper leveling of the coal

82 AMERICAN INSTITUTE^OF CHEMICAL EXCINEERS

in any oven is a matter of great importance, and it is a source of
regret that so little attention is paid to this feature of the process
by the beehive oi)erators throughout the country. With improper
leveling, the different heights of charge become coked to the bot-
tom at different periods of time, thus exposing the top surface of
the coke to the prolonged action of the air admitted for the
completion of the process, with a resultant loss of coke, or if the
process be stopped short of completion the coke from the higher
portions exhibits black butts.

LONGITUDINAL OVENS

The decreasing efficiency and scarcity of labor and the increased
cost of coking coal has led to experiments to reduce both of these
factors, first by making the coking operation non-dependent on
large numbers of laborers, and secondly by decreasing the cost
of actual operation. From these experiments was evolved in
1906 the longitudinal oven (a modification of the old Lielgian type),
with its mechanical devices for leveling, pushing and loading of
coke. Figure 3 shows a section of this type of oven and the method
of operation. In its essential details it may be described as a long,
narrow, rectangular chamber generally somewhat larger at the
discharging end, with sloping barrel roof approaching the center
from both ends, a trunnel-head in center of roof, flat tile bottom
and doors the whole width of the chamber at either end. These
ovens are placed side by side forming a block and are charged as
in beehive practice, from a larry running on a track supported on
the ovens. The oven is drafted from both ends, after the method
of the beehive oven, and the coke, after being watered on the
inside of the oven, is pushed out by means of a pusher, devised for
the purpose, onto a traveling conveyor, which transfers it to cars ;
screening being more or less fully accomplished during the passage
of the coke along the conveyor. During the last three years this
type of oven has come into prominence, especially in the Lower
Connellsville region, and many claims are made for it in regard
to increased yield, better product, lower cost of production, etc.,
but judgment must be withheld until these ovens have been in
use for a longer period and prove their worth by actual service.

BEEHIVE COKE OVEN INDUSTRY OF THE UNITED STATES 83

o

§

IT
U
CL

Z o

Q UJ

o Q

o

X
CO

o

F
O

u
c/)

84 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

BEEHIVE OVEN WITH ARRANGEMENT FOR UTILIZING
WASTE HEAT OF GASES

Waste heat from beehive ovens is utilized at some few plants in
this country for the generation of steam. The ovens, either bank
or double-row, are provided with a tunnel, built in case of the bank
ovens directly behind, and the double-row between the rows, and
extending the whole length of the ovens to be used for this pur-
pose. From each oven a flue is provided leading from the oven
to the tunnel and so arranged that it can be dampered off. This
flue is placed in the crown of the oven above the height to which
the coal is charged. Numerous schemes for placing the flues lead-
ing from the oven to the main flue have been tried. The usual
practice is a short straight flue from the oven direct to the tunnel.
At the boiler end a large stack is placed to cause proper draft.
In operation the regular trunnel-head is covered and kept closed,
the gases passing through the flue into the tunnel instead of into
the open air as in the ca.se of the ordinary beehive practice. The
waste heat passes along the tunnel in the direction of the draft
chimney and through the boiler setting before passing out of the
stack. The temperature in these flues is very high (around
2700° F.) and the building of flues to withstand this heat is a
matter of much consequence. The temperature of the gases at the
boiler approximates 2000 ° P., and the gases are sufficient in amount
to generate from 12 to 20 horse power per oven. The ovens bum
hotter under these conditions due to the better draft on the ovens
than when burning into the air.

BEEHIVE COKING IN THE SEVERAL COAL FIELDS OF
THE UNITED STATES

Beehive coke is produced in five of the seven great coal fields
of the United States: Appalachian field in Pennsylvania, Virginia,
West Virginia, Ohio, Tennessee, Georgia, Alabama and Eastern
Kentucky ; the Eastern Interior field in Illinois, Indiana and
Western Kentucky ; the Western Interior field in Kansas, Missouri
and Oklahoma; the Rocky-Mountain field in Colorado, Montana,
Utah and New Mexico ; and the Pacific Coast field in Washington.

Pennsylvania has from the beginning of coke making in the

BEEHIVg COKE OVEN INDUSTRY OF THE UNITED STATES 85

United States maintained the supremacy as to production, and
the beehive oven coke from the Connellsville region is still consid-
ered the standard coke of the country. All other cokes from what-
ever section of the country are judged by comparison with this
standard. The coal from this region, with approximately thirty-
one per cent of volatile matter, seems to contain just the proper
amount and composition of this volatile and to be given off at the
proper temperature and time to produce a maximum yield of coke
ivith a minimum loss of fixed carbon during the process. Prac-
tically all the coal in this region is mined for the production of coke
and is charged into the ovens without any preparation whatever.
About fourteen per cent of the coal from other coking regions of
the State is washed before coking, and the coke produced is of
varying purity and physical structure. The table herewith shows
the range of composition of the Pennsylvania cokes :

Moisture 0.23 to 0.91

Volatile matter 0.29 to 2.26

Fixed Carbon 92-53 to 80.84

Ash 6.95 to 15.99

Sulphur 0.81 to 1.87

West Virginia coal is of exceptional purity and the coking

industry, although second in production, is mainly as an incident

to the furnishing of st€ani and domestic coal. More than sixty

per cent of the coal charged into the beehive ovens is slack and

less than ten per cent of it is washed. At those plants where

proper attention is given to preparation of the coal and subsequent

operation of the ovens themselves, a coke of superior chemical and

physical properties is produced. The quality of the greater amount

of West Virginia cokes is exceptionally good, but a wide variation

is still to be found in the chemical composition of the cokes of this

State as the following range shows :

Moisture 0.07 to 0.60

Volatile matter 0.46 to 2.35

Fixed carbon 95-47 to 84.09

Ash 4.00 to 12.96

Sulphur 0.53 to 2.26

The coke produced in Virginia is from coal in the southwestern
part of the State and is all from unwashed coal. In chemical and

86 AMERICAN ISSTITVTE OF CHEMICAL ESCI SEERS

physical properties it resembles tlic cokes from southern West
Virginia.

The cokes from the southern jjart of the Appalachian licit!,
comprising the States of Tennessee, Georgia, Alabama and Eastern
Kentuck)', are for the most part made from washed coal, the (|ual-
ity of coke is poorer and the ash and sulphur are high. The average
ash is in the neighborhood of 14 or 15 per cent, and often running
up to 16 and 18 per cent where proper attention is not paid to
preparation and coking. The Birmingham district of Alabama
produces a fairly large amount of good beehive coke, with an ash
content averaging 11 i)er cent, but such coke is the exception and
not the rule.

Range of composition of above coke:

Moisture 0.75 to 1.34

\'olatile matter 0.75 to i-.y5

Fi.xed carbon 91.20 to 77.81

Ash 7.30 to 18.90

Sulphur 0.58 to 1.77

Beehive coking operations in the States of Illinois and Indiana
are practically at a standstill. A few ovens for experimental
purposes have been built in these States and have demonstrated
the practicability of producing coke from some of these coals. The
coking possibilities of Illinois and Indiana coals is confined to small
areas, and beehive operations will hardly be established in these
fields.

Kansas, ^lissouri and Oklahoma have had poor success in the
production of coke and the total output from these States is very
small.

Practically all the coke from the States of Colorado and New
Mexico is made from coal previously washed and crushed before
charging into the ovens. A plant of 350 beehive ovens of concrete
construction is one of the novelties of this region. The ovens
proper are of the ordinary beehive type, 13 feet in diameter and
7^/2 feet in height, constructed of firebrick and tile. The ring
walls and wharf walls are of plain concrete, the battery walls and
larry track columns of reinforced concrete. The yield of coke is
reported above the average for the region and is believed to be due
in great measure to the concrete construction which prevents the

BEEHIVE COKE OVEN INDUSTRY OF THE UNITED STATES 87

entrance of excess air so common in cracks developed in ordinary
beehive construction. For details of this plant the reader is referred
to Mines and Minerals, February, 1910, pages 429 to 432. At
another plant in this region the ovens are provided with under-
flues which convey the gases from the coal under the oven bottom
to a large flue, back of the ovens, which carries it to the power-
house. This power plant furnishes all the power for operation of
the mines, for ventilation, electric haulage, coal washing and crush-
ing, and steam heat for the company buildings and electric lighting
for the entire community. The flues under the oven bottoms serve
to hasten the coking and prevent black ends. The operation requires
careful watching to prevent the coal from coking up from the
bottom as well as down from the top. When the bottoms become
too hot and this coking upwards does take place a distinct line of
demarcation, where the two operations meet, is seen over the whole
charge of coke.

The cokes of these States are uniforml)' low in sulphur, scarcely
ever exceeding .75 per cent, but the ash is high, averaging 16 per
cent.

The coals used for manufacture of coke in Utah are practically
identical in character with those of western Colorado, but exhibit
the surprising characteristic of losing their coking properties and
becoming non-coking if kept in storage for any length of time.

Montana produces a very small amount of coke, all of which
is used in copper smelters. Attention is called to the fact that the
only restriction placed on the coke is that the ash content shall
not exceed 20 per cent. This restriction is only complied with
when the coal is washed. An average analysis of this coke shows
18.00 to 21.00 per cent ash and over 2.00 per cent sulphur.

Washington is the only State west of the Rocky Mountains that
contains coking coal and the area within the State is small. All
the coke is made from washed and crushed coal and is of fairly
good quality. An average analysis of this coke follows :

Moisture

0.92

Volatile matter

1.50

Fixed carbon

79-58

Ash

18.00

Sulphur

0.52

ACTION OF DISINFECTANTS ON SUGAR
SOLUTIONS

By GEORGE I>. MEAD£. Grunx-rry, JLa.

Jiead at Joint Meeting itaV/i the Eighth International Congress of Applied
Chemistry, New York City, September 4-13. )gi2.

This work was started with the idea of determining the
efficiency of chloride of lime as a preservative for sugar solu-
tions. Later the experiments were extended to include the action
of formaline, ammonium, fluoride, and a commercial preser\'a-
tive of the cresol variety. The work was done at odd intervals
during the last six months under conditions which made an extended
investigation impossible. Therefore, the results are somewhat
fragmentary.

All polarizations were with alcohol — ^0% of 959* alcohol —
and a minimum of lead subacetate solution.

The addition of the disinfectant was effected by adding i c. c.
of a solution of proper concentration to 100 c. c. of sugar solution.
For instance "chloride of lime i : 10,000" means that i c. c. of a 1%
solution of chloride of lime was added to 100 c. c. of the sugar
solution. In the " control without disinfectant " i c. c. of sterile
water was always added to compensate for the dilution due to the
addition of the disinfectant in tlie treated samples.

Acidities are quoted in number of c. c. of N/io KOH necessary
to neutralize 10 c. c. of solution, phenolphthalein as indicator.

Sterilized flasks stoppered with cotton were used in all the
work.

Experiments I and II. Cane syrup from the Triple Effect
28° Be, was infected with a portion of a sucrose peptone culture
of bacillus vulgatus. The artificial infection was probably super-
fluous. The syrup was divided into 100 c. c. portions and treated

ACTfON OF DISINFECTANTS ON SUGAR SOLUTIONS 89

as shown. The formaline, i : looo, was employed as a comparison
since this is the commonest preservative and the ordinary dilution
used in sugar work.

Action of Chxorjde of Lime on Arttficiaily Infected Cane Syrups after Six
Days' Incubation at 35-37° C.

Original

Control, no disinfectant .
Chloride of lime, i : 100.

I : 1 ,000

I : 10,000

I : 100,000

Formalin, i : 1000

3Q-2

21.8
37 Q
30 !
40. 1

17.52
4-44

10. 16
564

7 5

3 3
o 7

4 6

8 5
7 4
6 5

IO-5
Sl.alk.
14.4
13-5
130
2.0

The chloride of lime used in this and subsequent experiments
contained 19.75% available chlorine.

The noteworthy point in both these tabulations is that the
treated samples in the majority of cases show greater deteriora-
tion than the untreated control. Platings and a microscopic
examination of the samples in Experiment II showed no growth
with Formaline i : 1000, so the deterioration in that sample must
have been due to the acidity. Chloride of lime i : 100 and i : lOOO
showed numerous organisms. No difference could be detected
between the control and chloride of lime i : 100,000 so far as the
bacterial examination went. It may be that the artificial infection
was a disturbing factor in these two experiments.

Experiments III .\nd IV. In Experiment III juice from sound
cane was treated and in IV juice from frozen cane. The incuba-
tion period was 65 hours in both cases. There was no artificial
infection in these or any of the subsequent experiments on solu-
tions taken from the factory.

Experiment \'. Two sets of samples of the same juice were
treated identically. One set was polarized at the end of two days,
care being taken to prevent contamination, and again at the end
of three days. The second set was polarized at the end of five

90 AMERICAN INSTITUTE OF CUEMICAL ENGINEERS

Action or Culorjde of Liue on Cane Joice 65 Hoints in Incubator at 35-37° C.

Original

Control, no disinfectant .
Chloride of lime, i : 200.

I : 1 ,000

I : 10,000

I : 20,000

I : 100,000

Formaline, i : 1000. . . .

8.4
45

95
91S

2-3S
I 94

o 93
3 26

I3-3

9 5
1.9

2.88

2 83
3-79

3 26
3 36
2-3S
4.06

30
12.0
0.3
2.9

9 5
10. o
10.8

3-2

days. In this experiment the incubation was at room tempera-
ture.

Action of Chloride of Lime on Cane Juice at Room Temperature (23-30° C.)

Polarizations only. Original juice = 9.75 Polarization.
3.2 Acidity.

After
2 Days.

After
3 Days.

After
S Days.

Acidity
After
S Days.

8.2

9-4S
8.90
6.30
6.90
8.25

7-4

9-30

8.55

1-5

3-8

8.:

S 85
8.8s

-I.2S

-1-75

4-2

7 OS

0 8

6 0

75

5 5
3 5

I : 100,000

The three sets of results obtained on cane juice (III. W and V)
.are consistent in that they all show a markedly greater deteriora-
tion in the presence of chloride of lime, i : 10,000 than in the
samples where no disinfectant is used. The acidities and invert
sugar determinations give no basis from which definite conclusions
can be drawn as to the manner in which the organisms have
acted on the sugar. Microscopic examinations and platings on
sucrose agar of the juice in Experiment \' after two days' incuba-
tion show both yeast and bacteria in profusion in the control, and
in chloride of lime i : 10,000 and i : 100,000. There were only a
few bacteria, all of the gimi forming type, in formaline i : 1000,
chloride of lime r : 200 and i : 1000.

ACTJON OF DISINFECTANTS ON SUGAR SOLUTIONS

91

The next five experiments dealt with the action of various
disinfectants. Chloride of lime, formaline, (containing 4090
formaldehyde), ammonium fluoride and a cresol compound
designated as " Commercial Disinfectant " were the materials
employed.

Cane juice was no longer available as a medium, so the raw
sugar washings of the refinery were diluted for the purpose.
These washings are the heavy syrups purged from the raw sugar
in the first steps of the process. Necessarily they are heavily
infected with all the organisms which are on the outside of the
raw sugar crystals.

Experiment VI. Action of various disinfectants on raw sugar
washings diluted to 15° Be., 90 hours' incubation at 33° C.

Original
Control, no Disinfectant

Pol. 21.8
3-S

Acidity 1.8 c. c.
19.S c. c.

Chloride of Lime.

Formaline.

Commercial Disinfectant.

Pol.

Acidity.

Pol.

Acidity.

Pol.

Acidity.

I : 200

8-5

go

I : 1,000

7 5

17,0

19.2

6.0

21.9

2.0

I : 10,000

1,8

21.5

0.0

17.0

0. 2

17.0

I : 100,000

1.6

21 .0

2. 2

20.0

2.4

20. s

Experiment VII. Action of various disinfectants on raw
sugar washings to 15° Be., 66 hours" incubation at 30°-33°.
Polarizations only.

Original Solution 22.2

Control, no Disinfectant 5.4

Chloride of Lime.

I : 200

I : 1,000

I : 10,000

I : 100.000

2-4

5.4

220
4 5

The chloride of lime used in Experiments VI and VII was
found to contain only 7-35% available chlorine.

92

A \f ERIC AX IXSUTUTE OF CUEiflCAL ENCIXEERS

Experiment \'III. Action of various disinfectants on raw
sugar washings, at 20° Be., after 2 and 3 days' incubation
respectively. Polarizations only.

Original Solution 27.0

Control, 2 days 10.7. 3 days, 5.3.

Ammonium
Fluoride.

Chloride of Lime.

Formaline.

Commercial
Disinfectant.

2 Days.

i Days.

3 Days.

3 D»ys.

2 Days.

3 Days.

2 Days. ! i Days.

1 : i.cxx)
I : 10,000
I : too.ooo

O.S
9.2
10. s

28
41
51

12 2
10. 2
12. I

6.1

4.6

6.1

256

12.2
84

25 I
67
32

25,4 ! 24. s
14 5 10.3

9 3 4.3

Experiment IX. Action of formaline on raw sugar wash-
ings, 20° Be. Four days' incubation at SS^-SS" C.

Sample. Polarization.

Original 30.9

Control, no Disinfectant 15.8

Formaline i : i ,000 24. i

1 : 5,000 16.7

I : 10,000 15.8

1 : 20,000 14.6

I : 50,000 1 1 .2

I : 100,000 16.2

Experiment X. .'\ction of various disinfectants on raw sugar
washings, 15° Be., 60 hours' incubation at 30°-35° C.

Original 24.1

Control 130

Chloride of Lime.

Ammonium Fluoride.

Formaline.

1,000

5,000

10.000

20,000

50,000

100,000

11. 8
II. 7
II 7
12.3

14-7
14.8
14.4

ig.6
18.2
16.7
10.6

12. 1

12 2

ACTION OF DISINFECTANTS ON SUGAR SOLUTIONS 93

Microscopic examination of some of the samples in Experi-
ment X showed yeasts and bacteria to be about equally numerous
in the control, in formaline i :5,ocxD and i :50,ooo and in Chloride
of lime, i: 10,000. Ammonium fluoride i: 1,000 showed yeasts in
abundance but few bacteria. All of the samples including forma-
line I : 1 ,000 contained much gas.

The foregoing experiments all show that the disinfectants dealt
with actually aid deterioration when present in sugar solutions in
small amounts.

Ammonium fluoride is employed in distilleries in the propor-
tion of 4-8 grams per hectolitre (about i : 10,000) for the purpose
of inhibiting the growth of butyric acid bacteria without prevent-
ing the development of yeast. The fluoride stimulates the
decomposing power of the yeasts when present in certain propor-
tions. ("Sugar and the Sugar Cane," Noel Deerr, page 367.)

Since the results witb other disinfectants were of the same
general character as those obtained with ammonium flouride, it
seemed possible that the action was similar, although microscopic
examinations had failed to indicate that such was the case.

Experiments ; WITH Disinfectants in Artificially Infected
Sucrose Peptone Solutions

The medium employed for these experiments was the same as
that described by Owen, "Bacteriall Deterioration of Sugars"
(Louisiana Bulletin No. 125).,

Peptone \ o. 10%

Sodium Phosphate 0.20

Potassium Chloride 0.50

The percentage of sucrose was varied in the different experi-
ments.

Experiment XI. One portion of a sucrose peptone solution
containing 10% sucrose was inoculated with a pure culture of
yeast ; a second portion with bacillus vulgatus. These solutions
were incubated for 24 hours. They were then transferred in 100
c.c. portions to sterilized flasks, care being exercised to avoid
contamination. Chloride of lime was then added in various pro-

94

AMERICAN INSTITUTE OF CDEMICAL ENGINEERS

portions. The "original polarization" is on the infected solutions
after the twenty-four hours' incubation.

Action of Chloride of Lime on Infected Sucrose, Peptone Solution (io%
Sucrose) 3 Days' Incubation

Yeast.

Bacillus Vulgatus.

S S

7.6

OS

2.9

S-2

Unable to clarify
0.9

— I.O

7-4
Unable to clarify
Unable to clarify

Experiment XII. Action of chloride of lime on infected
sucrose peptone solution (20% sucrose) 3 days' incubation.
Room temperature.

Yeast.

Bacillus Vulgatus.

Mixture of Yeast
and Bac. Vulgatus.

Pol.

Acidity.

Pol.

Acidity.

Pol.

Acidity.

16. 1

1.6

17.0

0.4s

16.4

Control, no disinfectant. . .

12. 1

13

31

0.6

12.2

13

Chlorideof lime, I : 200
I : 1,000
1 : 10,000
X : 100,000

iS-7
IS 0
11.9

12. 1

Neut.
0.4
I 40
1 .0

16.5
16.2

2.6

30

Neut.
0.2
OS
0.6

16. s

iS-4 •
12 3
II. 6

SI. alk.

SI. alk.
13
I 45

Experiment XIII. Another experiment using chloride of
lime with yeasts and bacteria was carried out in 30% sucrose
peptone. For the bacteria in this experiment a pure culture of a
gum-forming organism isolated from a Cuban raw sugar was
used. The organism corresponded in all particulars to the "Ba-
cillus D" described in Lewton-Brian and Deers' Bulletin on the
"Bacterial Flora of Hawaiian Sugars."

ACTION OF DISINFECTANTS ON SUGAR SOLUTIONS

95

Action of Chloride of Lime on Infected Sucrose Peptone Solution (30%
Sucrose). Three Days' Incubation. Room Temperature

Yeast.

Bacillus "D."

30.0

30.0

Control, no disinfec

tant T.

27.7

26.7
29.8
30.0
29.6

23-7
16 6

21.4
24 9

The experiments with yeasts and bacteria in pure culture with
chloride of lime gave results fairly consistent with those obtained
on solutions from the factory. There is nothing in these experi-
ments to indicate that the action of the chloride of lime is the
same as that of the ammonium fluoride. In fact the solutions
containing bacteria gave more positive results, so far as stimulating
action is concerned, than those with yeasts. The results are not
very conclusive however as the stimulating action of the chloride
of lime is not so marked (except in Experiment XIII) as it was
where factory solutions were employed.

Experiment XIV. Experiments with yeast and bacteria were
run using formaline as the disinfectant.

Action of Formaline on Infected Sucrose Peptone Solution (20% Sucrose)
after Two Days' and Three Days' Iincubaton Respectively

Original

Control, no disinfectant

I : 5 ,000

I : 10,000

I ; 20,000

I : 50.000

16.7

16. 7

2 days

12-5

3 days
9.8

days
4 5

3 days

3-4

16.7
14.4
13 8

iSS
II. 8

16. 7
16.6
16.7
51

16.6
16.4
iS-3
3-4

Experiment XV. Action of formaline on sucrose peptone
inoculated with a mixture of yeasts and bacillus vulgatus. At
room temperature.

96

AMERICAN ISSTITVTE OF CHEMICAL ESGISEERS

Yeasts and Bacteria
Mixed.

Original

■5 95

2 Days' Incubation.

3 Days', Incubation.

7-7

4 25

12 4

10 3

11 5
9 2
9 5

9 7°
6 8o

8.2

5 4
5 6

The two experiments with formaline in artificially infected
sucrose peptone solution failed to show any stimulating action
whatever.

In order to see whether the unsatisfactory results so far
obtained with infected sucrose peptone solutions were due to the
inoculation or to the medium, four experiments were carried out
as follows: —

Sucrose peptone solution in lOO c.c. portions was infected with
one c.c of a io% solution of raw sugar washings such as had
been used as a medium in previous experiments.

Experiment XVI. Action of formaline on sucrose peptone
solution (30% sucrose) infected with I'i of a lo'/t raw sugar
washing solution, 30°-33°C.

2 Days' Incubation.

4 Days' Incubation.

Acidity at End of
4 Days.

Control, no disinfectant ....

10 I

10. 2

17.0 r.c.

Formaline, i : 5,000

I : 10,000

I : 20.000

I : 50,000

I : 100,000

I : 200,000

2.S.5
23 5
10. 7
20.0
IQ.2
107

104
15.8
12.3
12.5
10.8
II. 9

5 8
6.8
40
17.8
ig.6
14 7

Experiment XVII. Action of various disinfectants on sucrose
peptone (30'^ sucrose) infected with i7( of io7f solution of raw
sugar washings. Four days' incubation. 30°-33° C.

ACTION OF DISINFECTANTS ON SUGAR SOLUTIONS
Original ^28.2.

97

Amm. Fluoride.

Formaline.

Chloride

of Lime.

Pol.

Acidity.

Pol.

Acidity.

Pol.

Acidity.

Control, no

disinfectant . . .

25-3

31

25-3

31

253

31

1 ,000

27.8

1.8

28.6
259
24.9
24.7
23-8

21-5

0.8
1.9

2. I
2-S
2-4
2.Q

28.2
26.8
22. S
26. s

0, 2
4.4

4-4
5°

21-5

3 2

18.0

3-2

Experiment XVIII. Action of various disinfectants on sucrose
peptone (so'/t sucrose) infected with i^/i of 10% solution of raw
sugar washings. Three days' incubation. 30°-35° C.

Original ==28.3.

Amm. Fluoride.

Formaline.

Chloride of Lime.

Control, no disinfectant ....

27.9

27 9

27.9

1,000

S ,000

28.3
25.0
24.8

28.0

27.0
27-4
28.6

26. s
27-S

Experiment XIX. Action of various disinfectants on sucrose
peptone (20% sucrose) infected with i^^ of lo^c solution of raw
sugar washings. Three days' incubation at 33°-35° C.

Original :=20.2.

Amm. Fluoride.

Formaline.

Chloride of Lime.

Control, no disinfectant. . . .

17-5

17.5

175

20.2

18. 1
13-3

20. 2

20.0
18.9
18. I
18.7

5 ,000

19.4
173

98 AMERICAS' INSTITUTE OF CHEMICAL ENGINEERS

Of the four experiments with sucrose peptone inoculated with
a small portion of raw sugar washings, two gave results of the
same class as those obtained while working with solutions from the
factory, while two failed to give such results.

If time had permitted, experiments of the same character as those
just recorded, varying the reaction and composition of the medium,
the time and temperature of incubation, and various other factors,
would have been carried out. This class of work might have given
an insight into the conditions under which the stimulation by the
disinfectants takes place most readily.

In order to show that there is no chemical action on the part of
the disinfectants themselves, sterile sucrose peptone solutions, to
which had been added ammonium flouride i : looo and chloride of
lime I : lOOO respectively, were kept in the incubator at 38° C. for
three days. No change in polarization was observed in either
solution.

SuMM.ARv OF Results

I. Chloride of lime, ammonium flouride, formaline and the
cresol disinfectant, when present in sugar solutions in small amounts
varying with the disinfectant and with undetermined conditions
cause a markedly greater deterioration than occurs in untreated
samples. '

II. Experiments with chloride of lime in pure culture of yeast
and gum-forming bacteria indicate that the stimulation occurs in the
case of both organisms.

III. Ammonium fluoride one part to one thousand parts of
sterile sucrose peptone and chloride- of lime in like proportion
caused no change in the polarization of the solution during three
days' incubation at 38° C.

Note. — Since the foregoing paper was submitted to the Congress there
has come to my notice an article by Hugo Kiihl in Pharmazeutische
Zentrallhalle, Vol. 52, pp. 1316-1317, which has direct bearing on my work.
The article is a review of the results of investigations by various men
which show that very dilute solutions of poisonous antiseptics increase
the growth of bacteria, yeast, moulds and plant life generally. An abstract
follows :

Formaldehyde, i :500.ooo in milk gave a vigorous growth of penicillium
glaucum in five days. Without the formaldehyde there was only slight
growth in eight days.

ACTION OF DISINFECTANTS ON SUGAR SOLUTIONS 99

Ono found that forty parts per million of copper sulphate doubled the
mycelia of aspergillus niger formed in sugar solutions. Zinc sulphate in
amounts varying from two parts per million to one hundred sixty parts
per million increased growth also.

Shultz showed that mercuric chloride, chromic acid, formic acid and
salicylic acid in very small amounts stimulate the growth of yeasts. For
example, mercuric chloride I : 500,000 gives distinct stimulation. These
poisons also stimulate bacterial growth.

In large quantities the action is inhibitory ; in very minute quantities
there is no action ; between these two extremes stimulation occurs. The
line of demarcation is not sharp. The amount of stimulation and the dilu-
tion at which it occurs is dependent on the presence of other substances.
Increase of temperature increases stimulation.

The reason for this stimulating action has not yet been determined.

THE DECOMPOSITION OF LINSEED OIL DURING
DRYING

Il> J. C. OLSEN and A. E. RATNER

Read at the Joint Meeting with the Eighth International Congress of
Applied Chemistry. Neiv York, September 4-13, 1912.

There are various statcmenls, in the hterature on hnseed oil,
that during the ])roces.s of drying carbon dioxide is given off. The
authors have failed to find the record of any definite experiment
indicating the amount of this constituent which is evolved during
the drying process. No definite information could be found with
reference to the amount of water evolved. Experiments have been
conducted to ascertain the increase in weight of linseed oil during
drying, the assumption being that this increase in weight is due to
the absorption of oxygen. It is evident that, if volatile constituents
are given off during the drying process, the increase in weight will
not give a true measure of the oxygen absorbed.

In order to secure more definite information with reference to
this very interesting and important reaction, an experiment was
carried out in which pure, dry air was conducted over a weighed
amount of linseed oil. The increase in weight of the linseed oil
was ascertained and the moisture and carbon dioxide given oflf were
absorbed and weighed so that the total amount of oxygen which
combined with the linseed oil could be calculated.

The linseed oil used for this purpose was a sample of the oil
prepared under the direction of Committee E of the Society of
Testing Materials. Four samples were prepared under the direction
of this committee under conditions which seem to absolutely
guarantee that the samples taken were pure linseed oil. Four
samples were received from Mr. G. W. Thompson, sealed and
packed exactly as they were sent out by this committee for analysis.

The full description of the method of preparing these samples,
as well as the analysis, may be found in the report of Committee

100

THE DECOMPOSITION OF LINSEED OIL DURING DRYING 101

D of the Society of Testing Materials. The sample upon which
our experiment was conducted was pressed from the seed by the
National Lead Company, April, 1909. On the 25th of April, 1912,
when our experiment was begun, the oil was clear but there was a
slight sediment in the bottle. The bottle was thoroughly shaken
when the portion experimented on was weighed out.

5.336 grams of the linseed oil was transerred to a weighed
Florence flask of 400 c.c. capacity. In order to expose this large
amount of oil in a thin film to the gases of the air 3.8666 grams of
glass wool were placed in the bottle. By previous experiment, this
amount had been found just sufficient to soak up the oil after the
walls of the flask had been covered by a thin film. A similar flask
was used as a counter-poise in all the weighings so as to eliminate
the error due to air displacement and films of moisture on the
surface of the glass.

The flask containing the linseed oil was connected up in a series
of tubes as follows. A glass tube extended into the open air so as
to avoid acid fumes and impurities from the laboratory air. The
air was first passed through a large tower containing soda lime
and caustic potash in lumps, then through a Geissler bulb containing
strong caustic potash solution ; then through a U tube containing
concentrated sulphuric acid and glass beads. The air thus freed
from carbon dioxide or other acid gases and water passed into the
flask containing the linseed oil through a tube extending to the
middle of the flask. The exit tube passing out from the upper part
of the flask conducted the air into a weighed U tube containing
concentrated sulphuric acid and glass beads; thence into weighed
Geissler bulbs containing strong caustic potash solution ; then
through a weighed U tube containing concentrated sulphuric acid
and glass beads ; then through another sulphuric acid tube to an
aspirator, holding 7.5 liters. This aspirator drew 7.5 liters of air
through the apparatus at night and 7.5 liters during the day ; the
flask containing the oil, the sulphuric acid tubes, and the Geissler
bulb being weighed morning and evening.

Before the experiment was started, the apparatus was tested
over a long period of time by drawing air through in the manner
indicated, and weighing the tubes night and morning until it was
certain that all sources of error had been eliminated and that the
various weighed tubes had become constant. The flask designed

102 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

for the linseed oil then received its charge of weighed linseed oil,
and the experiment continued for 74 days. The results of the
experiment are given in tabular form.

The determinations bracketed are doubtful on account of slight
errors such as spattering of the li(]uid in the tubes, etc. Table II
was calculated from Table I by adding together the daily increases
in weight, so that the figpares given for each day give the total
quantity on that day. Table III was calculated from Table II by
dividing the various quantities by the weight of oil taken, 5.366
grams.

It will be noted that moisture and carbon dioxide were given
off almost immediately in fairly large quantity. The oil which was
slightly yellow in the beginning soon became colorless and gradually
acquired a dark yellow color. Volatile matter also began to be
evolved from the linseed oil. This was ascertained from the
observation that small oily drops collected in the neck of the flask.
The weighed sulphuric acid tube also gradually acquired a brown
color which ultimately became black. This would, undoubtedly,
produce an evolution of sulphur dioxide, which would be absorbed
by the caustic potash solution in the Geissler bulb. Only toward the
end of the experiment did the sulphuric acid tube which follijwed
the Geissler bulb acquire a dark color. It is reasonable to suppose,
therefore, that little, if any, volatile matter escaped absorption and
that, therefore, while the increase in weight of the absorption tubes
does not correctly represent the amount of water and carbon dioxide
evolved, it does represent the total volatile matter given off by
the oil, so that the increase in weight of the oil, plus the increase
in weight of the absorption tubes rejjresents the total amount of
oxygen absorbed by the oil, and that experiments in which only the
increase in weight of the linseed oil film is noted, do not represent
correctly the amount of oxygen absorbed. On the accompanying
plate, a curve is drawn representing the amount of oxygen absorbed
in the reaction. This was obtained from the increase in weight
of the oil, plus the increase in weight of the absorption tubes.
Another curve is given, showing the amount of water evolved, and
another one showing the amount of carbon dioxide evolved. The
accuracy of these curves and more especially the one representing
the amount of water evolved, is vitiated by the fact that a volatile
organic substance was produced. This volatile substance, however,

TBE DEtCOM POSITION OF LINSEED OIL DURING DRYING 103

TABLE I
Daily Record of Weights Taken

Carbon Dioxide

Given Off,

Grams.

ist. .

2d..
3d...
4th..
Sth..
6th..
7th.
8th.
9th.
lolh
nth
1 2th
13th
14th

ISA
i6th
17th
i8th
19th
20th

2ISt.
22d.
23d.
24th

2Sth
27th
28th
30th
32d.
3Sth
38th
41st.
44th
48th
Sist
S3d.
S7th
62d.
74th

0.0254
0.0060
0.0044
0.0060
0.0102
0,0140
0.0178
0.0286
0.0276
0.0156
0.0374
0.04 54
0.0274
o . o6g6
0.0796
0.0756
0.0650
o , 0478
0.0600
0.0636
o . 0408

0.0354

0.0400
o 0184

O.OII2
O.OII4

o 0108

O-OI56
0.0064
0,0082

o 0058
o 0092
o 0071
o 0054
o 0058
o 0040
0.0032
0.0012

O.OOII

o . 0306
0.0155
0.0236
o . 03 1 6

0.0088

0.0II8
o 0334
0.0164
0.0218
0.0102
0.0292
o 0364
o 0202
0,0438
0,0246
0,0200
0.0098
0.0156
0.0230
o 0150
0.0270
0,0212
0,0560
0,0272
o 0356
0,0268

0,0088

0.0260
o 0304
0,0202
0,0130
o 0046
o oobi

0,0057

0,0072
0,0086

0,0043

0,0068

0,0156
0.0106
0.0138
0.0244
o 0270
0.0124
0.0080
0.0038
(0.0084)?
0.0128
o 0094
0.0072
0.0063
0.009s
(0.0074)?

o 0054
0.0000
o 0078
o 0066
0.0042
0,0058
0,0056

(0,0056)?

o 0057
0,0079
o 0052
o 0010
o 0090

O 002 2

0,0078
0,0028
o 0028
o 003 s
0,0038
0,0018
o 0026
o 0020
o 0025
0.0007

104

AMERICAN INSTITUTE OF .CUEMICAL ENGINEERS

TABLE II
Total Amount of Quantities Determined

Increase in

Weight of Oil

Lirams.

Water Given

Off.

Grams.

Carbon Dioxide

Total Oxygen

Absorbed.

Grams.

ISt . . .
2d...

3d-.-.

4lh . . .

Slh...

6th...

7th...

8th...

9lh...

loth 1 .

nth. .

i2th. .

13th..

i4lh. .

iSth..

i6th.

I7lh. ,

18th .

19th.

20th.

2ISt. .
22d. .
23d..
24th.

2Sih.
27th.

28th.
30th.

32d. .
35th.
38th.
41st.
44 th.
48lh.
Sist.

S3d-.
S7th.
62d..
74th.

o 0254
o 0314
0.0358
0.0418
0.0520
0.0660
0.0838
o. 1124
o. 1400
o 1556
0.1930
0.2384
0.2658

o 3354
0.4150
0.4906
0.5556
0.6034
0.6634
0.7270
0.7678
0.8032
0.8432
0.8616
0.8728
0.8842
0.8950
0.9106
0.9170
0.9252
0.9310
0.9402
o 9473
o 9527
o 9585
0.9625
0.9657
o . 9669
0.9680

o 0306
0.0462
0.0698
o 1014

O II02

o. 1220
o 1554
o 1718
0.1936
o . 2038
0.2330
0.2694
o . 2896
o 3334
o 3580
0.3780
o 3878
o 4034
o 4264
o 4414
o 4684
o 4896

0.5456

o 5728
0.6084
o 6352
o 6440
o 6700
o 7004
o. 7206
o 7336

0.7382

o 7443
o 7500
0.7572
0.7658
0.7701
0.7769
0.7821

0.0156
0.0262
0.0400
0.0644
o 0914
o. 1038
0III8
O . 1 1 56
o . 1 240

0.1368

o. 1462
o 1534
o 1597
o. 1692
o. 1766
o 1820
o. 1820
o . 1 890
o. 1964
0.2006
o. 2064

0 . 2 1 20

o. 2176
0.2233
0.2312
0.2364
o 2374
o . 2464
0.2486
0.2564
0.2592

0.2620
0.2655
o 2693
0.27II
0.2737
0.27S7
0.2782

0.2789

0.0716
0.1038
0.1456
0.2076
0.2536
0.2918
o 3510
o 3998

0.4576

o . 4962

0 5722
0.6612

0.7151
0.8381

o . 9496
I .0506

1 1254
I 1958
I . 2S62
1.3690
I .4426
I . 5048
1 .6064

I 6577
I. 7124

1.7558

I 7764
1.8270

1.8660

1 .9022

1.9238
I 9404
I 9571

I .9720

1 9868

2.0020

2 0115
2.0220

2.0290

TBE DECOMPOSITION OF LINSEED OIL DURING DRYING 105

TABLE III
Total Amount of Quantities DETERisuNED in Percentage of Oil Taken

Increase in

Weight of Oil.

Per Cent.

Water Given

Carbon Dioxide

Total Oxygen
Absorbed.
Per Cent.

ist.
2d..
3d..
4th.
Sth.
6ih.

7th.
Sth.
gth.
loth
nth
1 2th
13th
14th
I Sth
1 6th
17th
I Sth
19th
20th

2ISt,
22d.

23d.
24th
2Sth
27th
28th
30th
32d.
3Sth
38th
41st
44th
4Sth
Sist,
S3d.
S7th
62d.
74th

6

67

7

05

7

21

7

S°

7

«4

8

23

8

72

Q

20

10

18

10

67

II

30

II

80

12

00

12

50

13

05

13

41

13

66

13

73

13

82

13

95

14

10

14

26

14

35

24

00

25

50

2b

95

28

00

20

50

30

90

31

90

32

70

33

10

34

00

34

80

35

5°

35

80

36

20

36

5°

36

80

37

00

37

30

37

io

37

h

106

AM ERICA. \ JXSTITL'TE OF CHEMICAL ENGINEERS

1

ft

3

iS

U

e:

.

'8

e

S

,

%4

>
,5

>

5

2

s

o

3

^

5

9

-^5

—

1

B

.

S

I

1

1

I

S

1

u

S

\

1

\

'

o

\

i

r

4

k

\

\

•a

VN

^

\

\

,

^.

'

\,

\

n

x

^

s

\

N,

\

\

^^

N

\

\

n

o

A

Ib^

N

\

. \

Q

fe

Q

N

*

k\\

o

o

in

\

1,

\

o

/5

\

^

\

u

L_

_J

bnsusj^

THE DECOMPOSITION OF LINSEED OIL DURING DRYING 107

is probably high in hydrogen, and an attempt will be made in the
future to isolate a larger quantity of this constituent and identify it.

The composition of linseed oil is generally given as follows:
Carbon 76 per cent; Hydrogen 11 per cent; Oxygen 13 per cent.

Neglecting the error due to the volatile oil given off, the linseed
oil lost 1.87 per cent of its carbon and 14.73 PS'' cent of its hydrogen.

At the time this paper was written, the flask and the absorption
tubes had not yet become constant in weight. The experiment
will be continued until constant weight is obtained.

It was believed that the results, though incomplete, were of
sufficient interest for publication.

TESTS ON THE OPACITY AND HIDING POWER
OF PIGMENTS

By G. W. THOMPSON.

Read at the Detroit Meeting, December 4, 1912.

In the discussion of paint problems, certain terms are often
used with such different meanings that great confusion has resuhed.
Thus the phrase "covering power" is defined in three or more dif-
ferent senses by Dr. Dudley in his articles in the Railroad and
Engineering Journal running in the issues of 1890 to 1893; and tiie
word "body" has so many different meanings that hardly two
persons consider it as referring to the same thing. For this reason
it seemed desirable to Committee D i of the American Society for
Testing Materials that the use of these two terms should be dis-
couraged ; and they have substituted two simpler terms to cover the
more usual uses of these words. These terms and their definitions
are as follows :

Hiding Pozcer: The power of a paint or jiaint material, as used,
to obscure optically a surface painted with it.

Opacity : The obstruction to the direct transmission of visible
light afforded by any substance, comparison being made with sec-
tions of equal thickness. The opacity in the case of pigments should
be considered as referable to their opacity in a vehicle under standard
conditions.

The distinction between opacity and hiding power should be
evident in the study of these definitions. Opacity refers to tests
made under standard conditions ; and hiding power refers to tests
made of paints, etc., as they are used. The distinction becomes
clearer when considered with reference to a paint the opacity of
which is measured with a standard thickness of paint, while in the
case of the hiding power the thickness of the paint will vary accord-
ing to the spreading rate at which the paint is applied.

In many laboratories tests for opacity have been conducted

108

TESTS 0.\ THE OPACITY AXD HIDING POWER OF PIGMENTS 109

on the assumption that what is known as the strength or tinting
strength of a pigment is a measure of its opacity. From numerous
tests which we have made we have come to the conclusion that
strength is an indication only of opacity, and that working on pig-
ments of the same composition, it is not safe to assume that the
strength of the pigment is a measure of its opacity. By strength
or tinting strength we mean here :

The relative power of coloring a given quantity of paint or
pigment selected as standard for comparison, which is the definition
agreed upon by Committee D i of the American Society for Testing
Materials. Much heated discussion has appeared in the Farben-
Zeitung during the last year or more as to whether strength is
proportional to opacity. Unfortunately, these discussions are
largely academic and not based on practical or accurate tests. As
far as the discussions go, it would appear that they have not led to
any definite conclusion. •

Without going into the question of the tinting strength of pig-
ments in this article, we propose to discuss a method which we
have developed for the measurement of the opacity of pigments and
paints which will serve, we hope, to some extent, at least, to clear
up one phase of this subject.

In developing a method for the determinations of the opacity
of pigments, it has been impressed upon us that opacity should
never be measured in terms of weight. This has been brought
out by Dr. Dudley and some of the disputants in the Farben-
Zeitung, but is not generally recognized as it should be. It seems
to us that there can be no question but that in all comparisons of
opacity, the relative volume of the pigment should be considered
and that a standard of opacity should be based upon a definite
volume of the pigment placed in a definite volume of a menstruum.
The futility of comparing pigments for opacity by weight is evident
where these pigments vary in their specific volumes as most pig-
ments of different compositions do.

In comparing pigments or paints for opacity, we are compelled
to recognize that it is somewhat of a physiological problem. We
really have no good means of detecting differences in light
except in the sensations they produce upon the retina of the eye.
Photochemical and photoelectrical methods have not so far proved
satisfactory. This being the case, all photometric work has to be

no AMERICAN JNSTJTUJE OF CHEMICAL ESCIXEERS

based upon certain standards for comparison. In the case of tests
for opacity, however, we have not as great difficuhy in this respect
as we have in the case of the ordinary photometric measurements.
By the use of a single source of light and a suitable photometric
bench, the opacity of a substance can be determined with a certain
degree of accuracy. Following the method used by Hiirter and
Drififield, who worked upon photographic plates, it is possible to
construct plates varying in opacity and whose opacity can be
determined. It is hardly necessary to describe in detail the method
to be followed for this work, and we would refer to the original
article by Hiirter and Driffield in the Journal of the Society of
Chemical Industry, \'ol. IX, 1890. page 455.

There is, however, one difficulty which affects the determination
of opacity and the preparation of standard opacity test pieces. In
a one light photometer the light is reflected so as to come from
opposite directions, and when properly balanced the light should be
equal at zero. By placing the object to be tested in the course of
one of these beams of reflected light, the light becomes reduced
and the balance of light is found at another point which gives a
means of calculating the opacity of the object being tested.
Unfortunately, the accuracy of the test depends upon no light being
reflected by the object being tested, or that the luminosity or reflect-
ing ])ower of the object being tested shall be determined and applied
as a correction to the opacity found.

Hiirter and Driffield worked upon gelatine silver films which
they apparently assumed had no reflecting power, or that, in their
case, the reflecting power could be included by them in the opacity
for the practical purposes for which tests were conducted. In the
testing of white paints, however, this cannot be assumed, for as we
will show, the amount of light that is reflected is apparently very
much in excess of the light that is absorbed during transmission.

According to the best information obtainable, opacity proper
follows a logarithmic law known as Bouguer's Law. Nutting in
his recent "Outlines of Applied Optics" — 191 2, says "Absorption
during transmission follows the logarithmic law in every known
case; that is, if a given layer absorbs a certain fraction of
transmitted radiation, the next equal layer will absorb the same
fraction." Thus, if the first layer absorbs half of the light being
transmitted, the next layer will absorb half of the remainder of

TESTS ON THE OPACITY AND HIDING POWER OF PIGMENTS 111

one-quarter of the light being trans-
mitted ; the next layer one-eighth of
the light being transmitted and so
on.

To express numerically the
opacity of a paint, we should define
in some term the light absorbed in
transmission for a standard thick-
ness. In a paper read before the
International Congress of Applied
Chemistry, J suggested that this
thickness be .1 mm. I find, how-
ever, that this thickness is too great
for the proper measuring of
opacity, and that it would be better
to use .01 mm. thickness as the unit
of thickness in which to express
opacity. Of course, any thickness
could be used, but it would be better
to have a thickness that corresponds
to some practical thickness of paint.
I, therefore, feel that it would be
better to adopt the latter thickness.
,In expressing the opacity it would
seem to me that it should be called
the "coefficient,'' and having the
coefficient we can calculate the total
opacity for any given thickness.
We would define, therefore, the
coefficient of opacity as the propor-
tion of light, expressed in a decimal
fraction of unity, absorbed during
transmission through a thickness of
.01 mm. of paint.

We have constructed a piece of
apparatus for the purposes of mak-
ing these tests which consists, first,
of a photometer which will bring
two fields of light into juxtaposition

Thompson's Opacimeter.

112 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

so that they can be compared by the eye. This photometer is placed
on top of two tubes, the lower ends of which arc covered with plano-
plano lenses. Below these lenses are two other similar lenses.
Below these are two total reflection prisms wliich direct light from
a series of incandescent lamps up tlirougii the tubes to the eye, and
by adjusting the prisms and the lamps, the light can be made to
be equally sent up through the two tubes. The tubes holding the
upper plano-plano lenses have on them micrometer milled wheels,
so that the distance between each set of lenses can be controlled
and measured. Paint placed between one set of lenses can be com-
pared with a standard paint or with a piece or pieces of paper w'hich
have been tested on a photometer bencli and the proportion of light
they transmit determined. The thickness of the paint can then be
varied until the amount of light transmitted matches that trans-
mitted through the standard paint, or the test papers. The thick-
ness of the film of the paint being tested is then read off on the
micrometer. Running another test with a different opacity standard
of paper or paint, two readings are obtained from which can be
calculated the amount of light that is absorbed and tiie amount of
light that has been reflected. Considering opacity as having to do
only with the light that is being transmitted, and not to do with
the light which is reflected from the surface of the paint, we can
figure tlie coefficient of opacity by the following calculation:

Let (ii = proportion of light transmitted by lest paper No. i.
(12= " " " Xo. 2.

fll <ll2.

6i = thickness of paint film transmitting the same amount of light as test

paper No. i.
62 = thickness of paint film transmitting the same amonut of light as test

paper No. 2.
Same paint formula is used for 61 and fcj.

c = incident light = unity.

:t = proportion of incident light reflected which is independent of the thick-
ness of the film except for very thin films.

Then -! = proportion of entering light transmitted by bi — bt thickness of paint,

02 being the light entering the 61— ij film, as it is the light transmitted
by the 62 film.

It Is necessary that we give here the development of a formula for the light that
passes through any number of units of thickness of paint:

TESTS OX THE OPACITY AND HIDING POWER OF PIGMENTS 113

/. = the light passing through any number of thickness units;
5 = the light absorbed by any thickness unit or units;
a = the light striking the first surface;

n = the number of units of thickness;

P = the constant opacity of each unit of thickness in the form of a decimal fraction
of unity.

Light passing through no unit of thickness:

Lo = a —a.

Light passing through one unit of thickness;

Li = a-Pa =a(i-P).

Light passing through two units of thickness:

U={a-Pa)-ia-Pa)P = aii-P)K
Light passing through three units of thickness:

L3={{a-Pa)-ia-Pa)P\-\{a-P<2-(a-Pa)P\P = a{i-Py.

Ln= aU-P)".

a

An=(i — P)"- General formula.

B„=i-A„=i-(i-P)''.

From the formula An=U — P)", where An is the proportion of entering light
transmitted, P is the opacity of unit thickness in terms of decimal of unity, and «
is the number of imits of thickness.

.^^^

From formula £»=! — (i— P)", where Bn is the proportion of entering light
absorbed.

b..= ,-[.-(;t!«;i;)]'-.

114 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

1—4: = proportion of incident light entering In film,

I'>bi(i —x)+x-\-ai = c = i,

-[-(-t)J"!

{i—x)+x+ai=i,

[.-(V--^.)J"

x =

I- 1 I

This formula seems rather complicated, but in practice and by
the use of logarithmic tables the work is more simple than it seems.

The apparatus to which I refer reads to the ten-thousandth of
an inch ; and preferably should have been constructed with the
millimeter scale. It is a simple matter, however, to make con-
versions into the mm. scale.

In making these calculations it is to be observed that the com-
parison of the pigments having been made between glass surfaces,
the amount of light reflected from the adjacent surfaces of a paint
would probably be different from the light reflected from the sur-
face of paint which is adjacent to air. This is a controlling reason
why the reflected light should not be considered in calculating the
coefficient of opacity.

In testing pigments for their coefficients of opacit)', we have
followed the plan of mi.xing these pigmnets with linseed oil on a
standard formula of 25 per cent by real volume of pigment and
75 per cent by volume of oil. In some cases, this may be too large
a volume for the pigment, as, for instance, in the case of zinc oxide,
to handle conveniently in the a|)])aratus ; but if trouble is e.xperienced
a different fonnula can be used, comparing it with another standard
pigment on this changed fonnula.

This apparatus is somewhat new and we have not as many
results to report of work done tipon it as could be desired, and
what we |)resent here is simply for information; and so that the

TESTS ON THE OPACITY AND HIDING POWER OF PIGMENTS 115

subject will be more generally studied, we present here some deter-
minations made in this apparatus working on a number of white
pigments. It is not to be supposed that these tests represent
average pigments or that the results presented are for the purpose
of condemning any of the pigments tested. It is very probable that
the pigments upon the market of the kind described vary con-
siderably from the figures presented herewith.

The coefficients of opacity and the light reflected by the dif-
ferent white pigments tested on the formula given above are shown.

The values for P are the coefficients of opacity as defined
above. The reflection is the proportion of incident light reflected
and is expressed in decimals of unity.

ficient of
city, P.

Reflection

0671

° 935

0794

0 956

0645

0 964

0578

0 947

0136

0 969

0813

0 927

oigo

0.823

oogo

0 859

0030 ■

0 856

0102

0 793

0114

0.858

White lead— Dutch

White zinc — American process
White zinc — French process. .

Lithopone

Calcium carbonate

Basic lead sulphate

China clay

Asbestine

Calcium sulphate

Silica

Barytes

This work was done in the research laboratory of the National
Lead Co., and much of it with the assistance of one of my associates,
Mr. R. L. Hallett, to whom I tender thanks.

Discussion

President Baekel.-wd: The paper of Mr. Thompson is now open
for discussion.

Secretary Olsen : I would like to ask Mr. Thompson, if this 6^^
per cent for white lead is 6iV of the total light that goes through?

Mr. Thompson : It is the total light.

Secretary Olsen : That goes through ?

Mr. Thompson : That is in process of transmission.

IIG AMERICAN Ii\STITLTE OF CHEMICAL ESCISEERS

Secretary Olsen : So that in order to get the per cent of the
total light which passes through you had to use your other factor,

93-3?

Mr. Thompson: Yes, sir.

Secretary Olsen : So that it would be about .36 per cent or
about a third of a per cent of light goes through.

Mr. Tho.mpson: That is, for the coefficient.

Mr. B.xker: I would like to ask Mr. Thompson what proportion
of light goes through the linseed oil. if that can be brought under
this schedule ?

Mr. Thompson: We have not made tests on linseed oil; it could
not be brought in the test with this apparatus. We have to work
with so much thicker films that we would have to construct some
different method for determining the opacity or the coefficient of
opacity of the linseed oil.

Mr. Baker: I would like to ask you about the construction of
your films.

Mr. Thompson : These lenses are detachable, removable from
the apparatus. The upper ones are cemented into the upper
cylinders, or the expansion of the upper cylinders. The paint is
rubbed up as carefully as it can be done without grinding and
placed in a little lump, so to speak, on the detachable plate that is
shoved into place, and then the micrometer wheel is turned until
the two lenses approach contact, then on the other side is a paper
that has been found to transmit so much light, so you have a standard
proportion of light going through, or you can work with a standard
paint, whose opacity or coefficient of opacity you have determined,
and then by setting that at a standard thickness you can work
the other paint you are testing until the amount of light trans-
mitted in each case is the same as seen through the photometer.

Mr. Baker: Are these pigments as marketed?

Mr. Thompson: Oh. yes, these happen to be piginents that were
used in painting a test fence, which has been constructed at Wash-
ington, under the auspices of Committee D-i of the American
Society for Testing Materials. The pigments were ground under
the direction of the Committee at Pratt Institute. Of course, these
particular pigments were ground in the laboratory of the National
Lead Co.

Secretary Olsen" : You made no tests of the comparative

TESTS ON THE OPACITY AND HIDING POWER OF PIGMENTS 117

opacity of pigments ground fine, of course, so as to get any results
on that?

Mr. Thompson: No, I didn't want to bring that phase of the
subject in. It is a most interesting phase, and we have some work
just under way which will give some very, very valuable information
regarding the causes of opacity. We naturally think of opacity
as being something inherent in the object. Properly we should
tliink of it as due to the presence of non-homogeneous particles.
Thus some parts of opaque glass have a higher refractive index
than other parts. Apparently there is in the case of very fine
particles no such thing as this kind of opacity. Whatever the
opacity is it is due to the relation to the medium in which it may be ;
and we find this, that if the medium has the same refractive index
as a particle, then the mixture of the two will be transparent, and
that it is due to the difference in the refractive indices that opacity
arises. That is one factor in opacity. The next factor that we
know of is fineness. The finer the particles, the greater the
opacity. Now, whether there are other factors remains to be
determined. But, from some other work which we have done, it
would appear almost as though those two factors can be considered
the dominant factors in opacity with reference to paint and pig-
ments.

Dr. Ittner: I do not know very much about paints, but the
question comes to my mind whether the refractive indices of the
different pigments vary much among themselves. Dr. Thompson
says that the opacity depends largely upon the difference in the
refractive index between the pigments and the vehicle, and the
question that comes to my mind is if he had a paint which is made
up of two or more pigments, with refractive indices possibly widely
divergent from one another, or, as different as possible, whether
tliat would have an influence on the opacity which was appreciable,
or whether the difference would be mainly the difference between
one of the pigments and the oil itself.

Mr. Thompson: There is considerable difference of opinion on
one part of the question that Dr. Ittner has asked as to whether in
mixed pigments the optical properties are additive, or whether
they affect one another. From such work as I have done it would
appear that they were additive. Because, you take two paints, one
having a coefficient of opacity of six, say, and another paint having

118 AMEKJCAN ISSTITVTE OF CHEMICAL ENGINEERS

the opacity of two, and you mix them together in equal proportions,
you would have a paint that would have an opacity of four. But,
there are other elements which come in affecting the hiding power
which might make a paint mixture work under the brush very
differently and give a greater or a less actual hiding power.

The difficulty which arises in this subject has been a means of
determining the opacity of fine particles, and the refractive index
of fine particles. I have been trying for years to find some method
of determining the refractive index of these particles, but so far
have been unable to find such a method. We have some work
under way which indicates that we can determine it indirectly. We
thought we had a method of determining the refractive index, by dis-
covering that the refractive index bears a very direct relation to the
dielectric properties of an object, but as soon as we came to the ques-
tion of determining the dielectric properties, we found that was
harder than determining the refractive index, and we had to give it
up. Some give 2.0 as the refractive index of white lead, but where
the figure originated I cannot find out, unless by assuming that tlie
refractive index of the mineral cerusite corresponds to the refractive
index of white lead. The refractive index of some pigments, such
as barytes, are comparatively low, and nearly approach the refractive
index of linseed oil, which accounts for their low opacity.

A very interesting thing illustrating this is that calcimine, which
is made largely of calcium carbonate, when it is put on witii water
as the medium, does not cover at all until the water dries out. and
air becomes the medium; air having the refractive inde.x of i.o,
calcium carbonate having a refractive index of about 1.5, and
water a refractive index of 1.33 the difference becomes verv much
greater, and a correspondingly increased hiding power is given to
the calcium carbonate by the substitution of water by air.

CONTROL OF INITIAL SETTING TIME OF
PORTLAND CEMENT

By K. E. WARE.*

Read at the Detroit Meeting, December 4, 1912.

It is well known that Portland cement, as burned in the rotary
kiln, is so quick setting that it cannot be used without the addition
of some retarding material, such as gypsum or plaster of paris.
It is not necessary to make this addition of retarding agent when
dealing with the product of a set kiln, probably for the reason that
the cement contains the ash of the fuel as well as most of the
sulphur.

Occasionally there has been reported a cement of such a nature
as to be quick setting even after the addition of the regular amount
of retarder, and this paper is in the nature of a report on the
commercial manipulation of a 100,000 bbl. lot of such quick setting
clinker. The manufacturer was interested, first irt correcting the
material on hand, and second in establishing a routine of operation
that would prevent a recurrence of the trouble.

The setting and hardening of hydraulic mortars has been the
subject of considerable investigation, for it is self evident that the
quality of the set of a cement determines the ultimate strength
of the concrete of which it is a constituent.

Experimenters do not seem to agree very well as to the
mechanism of this setting, nor as to the factors that exert the
greatest influence during the time that the hydrolysis is taking
place. Consequently there is a diversity of opinion as to the
method to employ during the processes of manufacture or as to
what subsequent treatment the cement must undergo, in order that
the manufacturer may at all times put upon the market a cement

*Credit is due to L. C. Nodell and P. H. Chang for the experimental
work in connection with this paper.

119

120 AMERICAN ISSTITUTE OF CHEMICAL ENGINEERS

wliose behavior may be predicted, and whose qiiahty will show no
deterioration during long time storage.

The consensus of opinion seems to be that the initial set of a
cement is due to some action for which the aluminates are
responsible, or to which they at least contribute in a large measure.

Also it seems to be quite well agreed that the retarding action
of gy])sum is due, if not to the formation of a double salt with
the aluminates, at least to the fact that it slows down their
hydrolysis, and consequently delays the initial set of the cement.

It has been the writer's good fortune to have been, at various
times, connected with the operation of Portland cement plants
using materials abnormally high in alumina, and he invariably
found that it was impossible, under those conditions, to vary the
lime content of the cement over any extended range, without
precipitating trouble. If the lime was carried high (63-64 per cent),
the cement too closely approached the danger line of unsoundness,
while if it dropped too low- (60.5-61), the factory was troubled
with quick setting cement.

Quick setting cement resulting from such operation is not so
responsive to the retarding action of gj'psum as one more nearly
normal in composition. Sometimes it will be quick setting direct
from the grinding mills, while at others it will develop a quick set
after short storage. Quite often it will show a reversion to quick
set if an excess of gypsum is added. The writer had his attention
called to a condition where two sections of a plant were operated
with differences of 30 per cent in the g)'psum added.

None of the cases of quick set in the writer's operating experi-
ence ever developed serious difficulties, as the setting times were
watched very closely, and at a suspicion of trouble in the stored
material, a quick cement was mixed out with a slower one, and
preferably one having a tendency toward unsoundness, the combina-
tion seeming to remain perfectly stable and not require any further
additions of g)'psum.

Also at any indication of quick set in the material coming from
the mills, the lime in the mix was immediately raised, a procedure
that never failed to correct the trouble.

This seems to agree with the experience of Meade.* who states
that quick setting cements that have come under his observation

♦"Portland Cement," Meade, p. 416.

INITIAL SETTING TIME OF PORTLAND CEMENT 121

are low lime cements. He states also, that he has retarded the
set of plastered cements that have gone quick by addition of
calcium hydrate or even calcium oxide.

It seems to be, however, a direct contradiction to the statements
of Reibling and Reyes* who state that all quick setting cements
contain free lime, remain quick setting so long as the lime is in
the form of oxide, become slow setting as the lime hydrates, again
quicken when the hydrate changes at carbonate, and finally
become slow setting as the hydraulic constituents become inert
through long exposure.

In view of these interesting experiences with quick setting
cement, it was with considerable interest that the writer responded
to an invitation from a cement company who reported a large
stock of clinker as quick setting, and beyond the influence of the
ordinary corrective methods.

The clinker was the regular fall run, stored over winter, the
plant being one that operated on marl, and followed the usual
practice of burning a large stock of clinker during the late fall
months to supplement their stock for the early spring demand
which opens before the ice leaves the lakes from which they dredge
their supply of marl.

An interesting circumstance in connection with the problem
is that, although some cement ground in the late fall showed quick
setting, the majority of it was perfectly normal except that it
would not stand any large additions of quick setting material without
itself showing an earlier set. Inquiry developed the fact that this
quick setting cement was ground during a short period that the
kilns were out of operation, and that when the kilns were started,
the rest of the fall grind showed a normal setting time.

Experiments were run to try the effects of different added
materials, such as plaster, (instead of gypsum), hydrated lime,
calcium chloride, and acids ; but none of them seemed to be suc-
cessful in retarding the set.

At the same time other experiments were tried, along the line
of hydration, as recommended by Bamber.j These were highly
satisfactory, the cement ground from clinker which showed a set of

♦Philippine Journal of Science, igii, 207.
fConcrete and Const. Eng.. 1909 (4) igO.

122 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

3-5 miiuitcs under ordinary procedure, being slowed to 2^2-3 hours
when hydrated to the extent of less than 2 per cent.

It seemed to make little difference how this water was added,
as is illustrated by the following experiments :

The cement after grinding with the usual amount of gypsum,
was heateil in a closed tube, the idea being that the water resulting
from the dehydration of the gypsum might prove sufficient for the
hydration of the troublesome constituents. This proved to be the
case.

The clinker was heated to approximately 100° C. and ground
while hot, the result being the same.

The ground cement was dropped through a vertical tube through
which a small cloud of steam was rising. Subjection to this
atmosphere for even so short a time as that necessary for it to drop
through a tube thirty inches long was entirely sufficient to retard
the set.

Water to the extent of 3 per cent was added to the ground
cement, mixed rapidly by hand, and then placed in laboratory pebble
mill where it was mixed mechanically for a short time. The set was
delayed, but not so uniformly as by the other methods.

Water was sprinkled on the cold clinker as it was fed to the
grinding mills at the factory. This treatment was satisfactory
so long as the water supply could be kept constant ; but the mill
operators could not be depended upon to regulate the supply
properly, and the idea was abandoned as impracticable.

Steam was turned into the conveyor leading from the mills. The
results from this method were not depentlable, and the scheme was
dropped as being too uncertain to be safe to use.

The method that was finally adopted was that of heating the
clinker and grinding while hot. This method proved entirely satis-
factory for the treatment of the greater part of the quick clinker,
the remainder being left over until the kilns should be in operation,
when the old clinker was ground with the new, the new being
purposely not thoroughly cooled.

The adoption of this method was largely influenced by the
layout of the plant, which with the clinker pile lying alongside of
the kilns and for their full length, made it a simple matter to
send part of the clinker through one kiln, and mix it on its return
with a quantity of cold clinker. The gypsum used was thoroughly

INITIAL SETTING TIME OF PORTLAND CEMENT 123

wetted and added to the clinker just before it reached the mill
hoppers, these hoppers being kept only partially tilled in order
that the clinker might not have time to cool or to dehydrate the
gypsum before reaching the mills.

From a consideration of the plant, it was a simple matter to
explain the quick setting cement that was ground in the fall. As
the stock of clinker grew larger, there was left only one place to
discharge the kiln output, and that was at the part of the clinker
pile farthest away from the kiln discharge, a point (Which is
nearest to the mills. This meant that for at least the last few
weeks the mills were grinding hot clinker ; but for the few days
that the mills were operated while the kilns were off fire they would
be supplied with cold clinker, and so ground out a small amount
of quick setting cement.

The table of analyses shows four analyses of quick setting
cements, 1-4, and three slow setting cements, 5-7, from the factory
stock. The set 8-12 belongs to a series of laboratory cements made
from the same raw material, in an endeavor to establish the safe
limits for factory operation.

These experimental burns were carried out in a small experi-
mental kiln designed by Prof. E. D. Campbell*, and used by him
in all his work on the composition of Portland cement, and the
influences that effect its constitution and characteristics.

The clinker from these burns was carefully sorted, and all
material that showed any signs of underburning was discarded.
The good clinker was then crushed and ground with gypsum.

This set of analyses shows alumina in a fairly high percentage,
but fails to show why this alumina has such a decidedly quickening
effect under conditions not entirely accounted for by the composition
of the cement.

In an endeavor to locate some of the influencing factors, a few
further experiments were carried out.

Quenched clinker from these high alumina samples showed
quick setting if perfectly dried, but slow setting if only air dried.

Steam clinker when air dried showed a retarded set when ground
with plaster.

All cements that have come under observation develop quick
set when heated to 350-400° C. This includes a number of com-

*J. Am. Chem. Soc, 24, 248.

124

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

TABLE I
Control of Initial Setting Time of Portland Cement

Clinker.

No. I. No. 2.

No. i. No. 4.

No...

No. 6.

I.O

2-4

22.4
36
7 4

61.6
2. 1
0.74

2 OS

quick

30
22.7
4.0
6.6
59 8
23
I 83

213
quick

13

22.35
4-4
6.35

62. S
2.0
>.57
2.07

normal

0.4
24.9
4.8

7 3
61.7

Silica

Ferric o.xide

Alumina

21.4

S-i

6.4

61 .0

2-3

1-74

1.85

quick

22.0
3 9
70

6> 3
24
I 57

2.02
quick

SO3

I 54
I S

SiOj

R.0,

Set

"■

23

7

10

I

63

3

I

36

2

36

3 hrs.

No. 12.

Loss

Silica

Ferric oxide
Alumina . . .

Lime

Magnesia. .

SO3

SiOt

R.0,

Set

0.03
22.48

4.2

7.3
62.9

2.2

1.58

I 95
normal

2.4

24 9

24.4

II. 7

10.9

59 4

58.5

2. II

2.21

1.58

2.13

2.23

quick

quick

23 7

10.4
61.4

2.17

J 57

2.28

quick

1. 16
23 9
9.8

61.7
2.14

1 34

2 46
i\ hrs.

mercial samples of varying composition and compoimded from
widely different materials. Two commercial cements tliat had
been stored since 1899 and which were presumably in their last
stage of slow set, had their initial setting time decreased from
35^ hours to I minute. There was a loss in weight during heating
of only 0.15 per cent.

A cement with a setting time of 15 minutes was treated
alternately with water and heat and showed a setting time curve
as in Fig. i. At each stage in this addition of water and subse-
quent heating to 350-400° C, a sample of the material was strongly

WITIAL SETTING TIME OF PORTLAND CEMENT

125

ignited and showed losses corresponding to the dotted curve of
Fig. I.

From- a consideration of the curve it would seem as though the
water must have been present in two different conditions, for
although the cement showed a continuously increasing amount of
water, the set was not correspondingly slowed. This may be
partially due to the fact that the heated cement retained some water
in such a condition that it was not driven off when heated to 350°

6hr

A

A

A

J Time

6hr

/ \

A

—

—

—I

OSS

jn Ignlti

un

\\

4hr

i

A

,

\ •

A

IS

3hr

\

/

\

1 ^

A

/

\

/

\

/

,\

\

/

y

'

/
/

\

/

2hr

/

\

/

/\

V '

/

/

A

\

/

V
\

/

\

//

\V'

\\

/ ,

^\

\

/

A

A

/

f

Ihr

I

V

V

/

/

/ \

\

/

'

/

/

\

/

/

\

/

5%

ifo

2%

Fig. I. — Setting Time and Loss on Ignition of Cement.

C, in which condition the water did not seem to exert much
influence on the setting time.

In an effort to establish whether it was the gv-psum or the
cement that was affected by heat, a cement containing no gypsum
was heated and afterward mixed with the normal amount. It
showed a slow set.

Another sample of the same material, unhealed, was mixed with
gj'psum that had been heated. While it required a larger amount
to retard the set (5 per cent)* it showeld a normal setting time.

Any one of these slow setting samples would develop a quick
set upon heating. In the case of the cement carrying 5 per cent
dead burned gypsum, it required a much longer time of heating

*Meade and Gano, Chem. Eng., i, 292.

126 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

than in the case of those samples carrying the smaller amounts.
The times of heating varied from 6 hours to 48 hours in the
different samples. Dry slaked lime showed no appreciable loss of
water under the same conditions of heating.

The whole set of quick setting cements was tested for free
lime according to the microscopic method described by Prof. A. H.
White.* There seemed to be no indications of free lime.

Although it may be impossible to draw any definite conclusions
from this rather incomplete line of experiments, it seems to be
certain that in this instance, at least, the quick setting was not due
to free lime.

This experimental work is to be continued, in the hope of
gathering further data that may assist in clearing away the uncer-
tainties in regard to the role that alumina and gypsum play during
the initial setting of Portland cement.

University of Michigan,
Ann Arbor, Michigan.

*J. Ind. and Eng. Chem., 1909 (l), 5.

THE EFFECT OF "LIME SULPHUR" SPRAY
MANUFACTURE ON THE EYESIGHT

By JAMES R. ■WITHROW^

Read at the Joint Meeting with the Eighth International Congress of
Afflied Chemistry, New York, September 4-13, 1912.

About two years ago, the writer was called upon to take charge
of the installing of a "Lime-Sulphur" department for a manu-
facturer engaged in other lines of chemical manufacturing.
Preliminary to starting, industrial experimentation, a very thor-
ough laboratory study had been carried out for the manufac-
turer, by his regular chemist. This work reviewed in a most
capable manner about all the recommendations, which have recently
sprung into chemical and experiment station literature concerning
"Lime- Sulphur" preparation. As a result of this work a formula
was evolved, which was used as a basis for manufacturing
experiments. The laboratory experiments themselves were never
made in larger than five-gallon apparatus. The writer witnessed
from time to time these experiments or portions of them and at
no time noticed anything causing discomfort. The laboratory
assistant, who did most of the experimental work for the
company's chemist and was constantly in contact with the material
and its fumes, never noticed any effect or discomfort at any stage
of the laboratory work, which extended through several months.
To be sure, there was the ever present odor of hydrogen sulphide
or at least a similar odor. This was never offensively strong. At
no time was it so noticeable as to compel enforced ventilation.

The writer's business was to accept the work as completed in
the laboratory and transfer it to factory operation. The first
factory experimental runs were made on about a 12 barrel scale.
These experimental cooks were made to get factory scale data
for construction work and also to uncover any imforeseen operation

127

128 AMERICAN ISSTITUTE OF CHEMICAL ESGISEERS

difficulties. The product had a specific gravity, varying from 45° to
32° Be., depending on the purpose of the experiment. The
solution produced of calcium polysulphide or so called "Lime-
sulphur," contained about 25 per cent sulphur, and about the
equivalent of 10 per cent calcium o.xide, when the specific gravity
was about 33° Be. Twelve barrels of this product therefore
would contain 1625 lbs. of sulphur and the equivalent of 650
lbs. of lime.

The first few cooks aroused no comment from employees about
the building, which was a large one of four stories, beyond what
would come from persons unaccustomed to hydrogen sulphide-
like odors. In the course of the next week or two, however, the
weather had become quite cold and the normal ventilation by means
of the windows was much diminished, because of an effort to
keep the place warmer by closing the windows. Again no particular
effect was noticed at first. The "cook" digester was a steam
jacketed cylindrical tank roughly 5' x 5' and supplied with a cover
and a small ventilating pipe. This pipe was inadequate for proper
ventilation of tank and would have been useless anyway, for the
top of the "cook" tank was usually always open during the
experimental runs. This was for purposes of observation during
the experimental cooks. The man in charge of the cooks usually
stationed himself at the opening to become familiar with boiling
conditions within the tank, during the various runs under different
conditions.

Within a cook or two, after the w indows were closed to diminish
the cold conditions, the man in charge of the cook became aware
of a smarting sensation in and around the eyes. The eyelids became
red. The writer was constantly about the tank, but was only
occasionally at the tank opening and felt little or no discomfort,
though there was a slight burning feeling about the eyes. The
room became partially filled with condensed steam at times and
finally, about 8 p. m., during a run which was a little prolonged,
the writer noticed that the steam or vapor in the room was greater
than usual and that the incandescent electric lights had a halo of
some eighteen inches in diameter, when viewed through the fog.
The halo tended to have rainbow colors. An hour or two after-
wards, the writer found the same conditions as to fog and halo
to exist in his room in his hotel, and concluded that his eyesight

"LIME-SULPHUR" SPRAY MANUFACTURE ON THE EYESIGHT 129

was affected. Cold water was applied liberally and he turned into
bed and went to sleep at once. In the morning the blurred eye-
sight was about as bad as the evening before. The foreman, who
stood at the opening of the cook tank, had gone home at the end
of the run at the time the writer did. He was unable to report for
work next day. His eyes were much inflamed and were too sensitive
to light to open them. He said they pained and felt gritty under
the eyelids. He w'as back to work again in a couple of days. In
the case of the writer, with the liberal use of saturated boric
acid solution the blurred vision gradually returned to normal during
the course of a week's absence from the manufacturing operation.
There was a recurrence of the blurred effect at another time, which
almost rendered vision impossible, but it rapidly wore off and at no
time was there any pain. The foreman never again had an attack
after his initial e.xperience. None of the workmen were affected
after proper precautions were taken.

At one time, however, when a batch was being concentrated
by boiling down, the cover was thrown open to expedite evaporation.
In the same room some distance away, two workmen were barreling
off finished product. Both the foreman and myself were actively
engaged about the cook tank and were practically unaffected. Of
the two workmen mentioned, however, the thin one was very
much affected and said he suffered agony all night and next day,
while the corpulent one was entirely unaffected. Other workmen
were in and out during the cook, but none were affected. The
one of the two mentioned above as unaffected has, since starting
regular operation in the new plant and in fact during the rest of
the experimental runs, been in active charge cf the "cooks" and
has never become affected, beyond possibly slight reddening of the
eyes.

No one at all has been affected in anyway after the new
plant was installed with its ample facilities for ventilation. Inquiry
directed to other manufacturers disclosed similar experiences.
One manufacturer's experience was so bad that he at once knocked
one side out of his cooking room. This is undoubtedly effective,
but from the writer's experience unnecessary. All that is required
is a hood over the cook tank, which will carry all vapors out
doors, and a "cook" room which is high ceilinged and reasonably
well ventilated. Providentially the copious evolution of steam has

130 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

caused most plants to provide hood-covered tanks, thus avoiding
the unexpected trouble we are discussing.

A search of the literature of "lime-sulphur" available to the
writer found no mention of the effect on the eyes. The suggested
reactions to explain the action of sulphur on calcium hydroxide
and water, varied as they were, gave no clue to what might have
been the body which gave rise to the trouble. During a subse-
(|uent study of jjolysulphide literature in general, however, it was
found that Bloch and his pupils ( Ber. d. Chem. Ges., 41, 1961 ;
Am. Chem. Jr., 41, 155) had prepared polysulphidcs of hydrogen
of the formulas H.^Sj and H.jS,. The latter is formed by heating
the former and is easily volatile. The fumes of these polysulphidcs
are said to have a penetrating disagreeable odor and their vapors
attack the mucous membranes. Thorpe says their vapors attack
the eyes. (Diet. Applied Chem., 1893. 3, 699). They are decom-
po.scd by alkalies and therefore would not e.xist very long in the
lime-sulphur cook, but if they were being given off in mere traces,
continuous e.xi)osure of such fumes would naturally cause
discomfort.

Hydrogen sul]iliide itself, however, may have been the cause
of the trouble. It has been shown to be a product of the evapora-
tion of a solution of calcium polysulphidcs. (Divers, J. Chem. Soc,
1894, p. 284.) Hydrogen sulphide could not likely have been the
cause, excc])t the symptoms of H^,S poisoning recorded are only
the effects of sudden or brief exposure to large amounts of the
gas and that prolonged exposure to dilute H.^S would cause a
different series of violent symptoms. This latter assumption does
not appear probable for in such cases where H._,S was permitted
in the atmosphere of laboratories in small amounts, the usual
symptoms, only not so pronounced, were the result. The only
recorded .symptom of hydrogen sulphide poisoning observed in the
cases under discussion was the occasional occurrence of headache.
This was to be expected, since hydrogen sulphide was itself being
evolved to some extent.

It should be mentioned, however, that K. B. Lehmann (.^rch.
F. Hygiene. Bd. XIV, 1892, 135; Blyth, "Poisons, Their Effects
and Detection," 3d ed., C. Griffin & Co., London, p. j^) mentions
cases where "intense irritation of eyes, nose and throat" occurred
within five to eight minutes of exposure to a concentration of 0.3

" LIME-SULPHUR" SPRAY MANUFACTURE ON THE EYESIGHT 131

per thousand of hydrogen sulphide, but no affection of the sight
is mentioned even in this extreme case. In long exposure to lower
concentrations, such as would correspond with the case of hours
of exposure in lime-sulphur cooking, the action recorded is on the
respiratory tract. These symtoms appeared entirely absent in the
lime-sulphur cases as also were all the other common symptoms,
(except headache) such as muscular weakness, etc. A tendency
to conjunctivitis, a symptom of chronic hydrogen sulphide poison-
ing, may have been present in the case of the man in charge of the
cooks. He was the man, however, whose eyesight itself was never
affected. The writer has suft'ered at other times in the last six
years, most of the symptoms of slow hydrogen-sulphide poisoning,
due to inadequately ventilated, over-crowded and poorly arranged
university laboratories, but the symptoms in the lime-sulphur
experience were quite different. In fact the usual muscular weak-
ness and general depression as caused by hydrogen sulphide
were not experienced at all in the lime-sulphur manufacture. It
should be mentioned also, that the writer has been informed that
attendants at "sulphur" baths have had their eyesight temporarily
affected in a similar fashion. Volatile polysulphides may be present
in this case also, although they have not been proven to be present
to the writer's knowledge in either case. This would be an inter-
esting point for someone favorably situated to develop.

It seemed possible therefore that these hydrogen polysulphides
might have been the cause of the action on the eyesight of the
vapors from the boiling of a mixture of sulphur, lime and water.

It may be stated at this point that this indication of the
presence of hydrogen polysulphide in the vapors of the lime-
sulphur cooks might have an influence upon the solution of the
problem of the actual reactions involved in lime-sulphur prepara-
tions, a mooted question at the present time. The trouble with
the eyesight always came, when a batch was being concentrated
by evaporation before filtration and not during ordinary cooks.

It seemed worth while to record these facts as a warning, at
least, as to the serious dangers of lime-sulphur manufacture in the
absence of adequate ventilation. This is all the more necessary
since it is probable that attention has not already been frequently
called to the matter, because ordinary ventilation precautions, only,
are necessary to avoid all trouble, and therefore the average manu-

132 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

facturcr has not had the experience or it has appeared so seldom,
that the isolated affection of a workman now and again may have
been attributed to something else. It is worth noting also because
the mere occurrence of a cold spell of weather gave the opportunity
of experiencing this difficulty possible in lime-sulphur manufacture,
so that otherwise it might never have occurred at this plant or
only in such isolated cases as to lose connection between cause and
effect.

Laboratory of Industrial Chemistry,
Ohio State University,
June 20, 1912.

ACETYLENE SOLVENTS

By J. H. JAMKS

Read at the Detroit Meeting, December 6, 1912
Part I.— LABORATORY METHOD AND TESTS

The Laboratory tests made to determine the relative industrial
value of various acetylene solvents were carried out as follows :

The acetylene was made from the commercial carbide in an
ordinary "Carbide to water" laboratory generator. It was purified
to remove ammonia, sulphur compounds, and phosphorus com-
pounds, by passing through a purifying train consisting of the
following vessels in order: a 10 per cent sulphuric acid solution,
a 15 per cent hydrochloric acid solution saturated with mercuric
chloride, two towers containing approximately equal parts of a
mixture of bleaching powder and slaked lime, a tower containing
slaked lime, only, and finally was completely dried by passing
through two towers containing fused calcium chloride.

It is necessary in order to get as closely as possible at the
true figure for the absorption of this gas in any of its solvents,
that the gas be free from impurities, and that the solvent be of
the highest purity attainable. It has been demonstrated that the
solubility drops ofT rapidly when impurities are present, either in
gas or solvent. To get the highest commercial efficiency it will pay
to purify the gas and select solvents of highest purity. Care with
reference to the purity of gas and solvent is at present not given
the attention in this industry that it deserves.

The method in detail of carrying out this absorption test was
as follows :

A carefully measured volume of the solvent (usually 1.5 ex.)
was placed in an ordinary five-inch side neck test tube, fitted through
a two hole rubber stopper with a glass tube gas inlet and a thermom-
eter, the bulb of which was immersed in the solvent.

134 A.\fER/CA.y INSTITUTE OF CHEMICAL ENGINEERS

This tube with solvent was immersed in a freezing mixture
(ice and salt) and cooled to —18° C. or —19° C. before starting.
The purified gas circulated through a four foot coil immersed in the
freezing mixture, thus bringing the gas to temperature of the solvent.

The acetylene was bubbled through the absorption tube at the
rate of about one bubble per second, in fact the gas was passed
about as fast as is done in an ordinary combustion in the analytical
laboratory.

Since volatile solvents are appreciably vaporized during this
process of saturation, the exit gas and vapor in such case was
passed through an ordinary potash bulb containing 95 per cent
alcohol to catch the solvent which was later determined and proper
connection made on the volume of solvent actually used. In 12
minutes the amount of solvent usually taken is completely .^^aturated
with the gas at atmospheric pressure (the pressure and tempera-
ture being always noted). The exit of the absorption tube was
then connected to a similar tube two-thirds full of saturated
calcium chloride solution which in turn had been saturated with
acetylene. The calcium chloride was connected to an ordinary
Hempel measuring burette ( the liquid in the latter also being a
saturated solution of calcium chloride subse(|uently saturated with
acetylene).

The purpose of the calcium chloride was to absorb any solvent
vapor that might be carried out in the solution of the gas, and
which would otherwise be measured with the gas, giving too high
a result. The saturated calcium chloride solution has a very low
absorptive capacity for acetylene and it has been proved that it
condenses and absorbs completely the vapors in each of the
solvents tested. The efficiency of the saturated calcium chloride as
an absorbent for the vapor of the various organic liquids suitable
for acetylene solvents was demonstrated by boiling the solvents,
and passing the vapor into such an absorbent tube, when the
absorption was found to be complete. In several of the experiments
noted below evolved gas from the measuring burette was bubbled
back through a "potash" bulb containing 95 per cent alcohol, but
no trace of solvent was found, which, if present, would have caused
the gas reading to be too high.

This detail is mentioned here, because objection might be
raised to the readings obtained with volatile solvents on the ground

ACETYLENE SOLVENTS 135

that the gas would contain some of the vapor of the solvent,
making a volume greater than the real volume of the gas.

The gas evolution begins soon after the absorption tube is
removed from the freezing mixture. While the solvent was
saturated at — 18° C. usually, to guard against the possibility
of the solvent not being saturated at the place taken as the starting
point, the readings were not noted until the temperature of the
solvent had risen to — io° C. The gas evolved from a known
volume of solvent, saturated at — io° C. (since if gas is evolved
between — 18° and — io° it must be saturated at — io° .C), up
to 30° C. is then measured, the figure obtained being recorded in
each of the determinations noted below. The readings are given
as actually obtained under the pressure and temperature conditions
of the laboratory, and this gas volume is reduced to zero C. and
760 mm.

The reason for selecting —10° C. as a point at which the
absorptions were determined, was that in commercial practice, it
is very easy to cool the containers to this temperature. The 30°
C. figure was obtained for the reason that with this the behavior
of the solvent could be predicted in practical use, where the gas is
rarely evolved at a temperature above 30° C.

Part II.— LABORATORY RESULTS.

The work of Claude and Hess {Compt. Rend. 124, 626) had
shown that the absorption value of acetone far exceeded that of
any solvent studied previously, and some preliminary skirmishing
among organic liquids soon led to the view that the absorption of
acetylene in acetone and other carbonyl compounds is partly
chemical, in the sense that a chemical reaction or a partial reaction
took place between the molecules of the absorbent or solvent and
molecules of the acetylene. It is well known to organic chemists
that the carbonyl group is a very reactive point in the molecule of
many carbon compounds, in fact this indicates a condition of strain
between the carbon and the oxygen, and the ready reactivity here
is quoted in support of Baeyer's "Strain Theory."

Some French investigators, 10 or 12 years ago, working
with higher acetylenes, actually obtained compounds which were
addition products. The composition of the compounds that they

13G AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

Studied seemed to justify me in making the tentative statement,
that there is a chemical action here, and I believe there is possibly
a ring combination between the carbonyl carbon and oxygen and
the acetylene, because of the unsaturated condition existing between
the two carbon atoms of the acetylene.

With the conception then, that the carbonyl group is acetone
was the reactive point, and that a chemical action of some kind took
place, the solvents noted below were tested- The results established
pretty clearly that there is a close relation here between the
structure and the absorption capacity of a given compound for
acetylene althougli the figures obtained for methylal and acetal
would indicate that the "carbonyl theory" is not a complete enough
one.

There is also a relation in a given series, usually, between the
molecular weight and the absorptive capacity.

The figures obtained are arranged in the tables on pp. 136 and
137, the values determined for acetone and certain other organic
liquids by previous observers being given for comparison.

SUMM.\RV OF LaEOR.MORY ReSI'LTS.

A study of the figures obtained establishes pretty conclusively
that of all the licjuids that have been tried, those organic compounds
containing the carbonyl group are the best solvents for acetylene.
We must exclude the organic acids, as the presence of the free
hydroxyl liydrogen here seems to work counter to the chemical
action upon which the remarkable solubility seems to depend.
That the "carbonyl theory" is not satisfactory in every respect is
shown by the high figures obtained for methylal and acetal. This
peculiar action seems to require the assumption of quadrivalent
oxygen for an adequate explanation.

Further, the figures clearly establish that in a given series
the absorption of acetylene is greater the lower the molecular
weight of the compound. The above experiments had in view the
selection of a solvent that could be used industrially. Since the
esters and acetals are out of the question industrially, requiring
two and three molecular units per molecule of product, respectively,
it was decided to try some larger scale experiments with acetalde-
hyde. making comparisons with other solvents in commercial use.

ACETYLENE SOLVENTS

137

Solubility of Acetylene According to Previods Observers

Acetylene Dis-
solved by I Vol.
Solvent.

Acetone

Acetic acid

Alcohol

Benzoline (gasoline) .

Chloroform

Parafiin oil

Paraffin oil

Carbon bisulphide . . .

Olive oil

Carbon tetrachloride

0.48

Claude & Hess
Berthelot

E. Miller
Berthelot

Fuchs & Schifl
Nieuwland

Preliminary Work on Solubility of Acetylene

(Figures refer to volume absorbed at — 10 degrees C, but volumes are not reduced
to standard conditions.)

Acetylene

Solvent.

Boiling-point
of Solvent.

Dissolved by

I Vol. Solvent.

at —10° C.

Remarks.

Ethylidine cyanhydrin

183

2.8

Acetoacetone

137

10. 2

Benzophenone i g. dissolv.

in 23 c.c.acetophenone. .

vols, absorbed

Methyl propyl ketone

102

14.8

Bat vric aldehyde

74

10.3

Acroelin

52

22.6

A crystalline compound of
acetylene and acroelin
forms during absorption

Propionaldehyde

48.9

24.2

Acetaldehyde

21

54

Acetaldehyde 50% by vol. \
Acetone 50% by vol /

■36

42.2

Acetaldehyde 50% by vol. 1
Ethyl acetate 50% by vol. /

43

40.2

Acetaldehyde 50% by vol. 1

Propionaldehyde 50% by \

32

311

vol. J

138

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

Absorption Figures on Acetylene Solvents
(The averages in the last column represent absorption at — lo" C. per c.c. solvent.)

i ?J 1

Acetaldehyde C.P.

MethylalC.P

Acetal. C.P

Methyl formate

C.P

Do

Ethyl formate C.P.

Iso-amyl formate
C.P

Do

Methyl acetate
C.P

Do

Ethyl acetate C.P.

Iso-amyl acetate

C.P

Do

76

0.81

44

32 3
32-3
54 S
,54. S

123
123

57 5
57-5'i

77 |i

77

139

139

70

69
46
46

15 6
«S-9

61.3
6i.i
48.9
48.4

28.8
29

45

45 4
20.4

47
46
30 7
30.6

10.4
10.6

8l 40.8

5 40.7

6 32.6
8 32 3

46

SI 7

19.2

19 3

23
22

21-5

25-8
25 4
18.8

25 6
23 5
245
24.4

23.2
23.8

18.4
17.2

23 4
21.8

42.
41 4'
27.4^
27 4-

9 3
9 5

36 6
36.6
29.9
29.6

17 2
17 4

58.8
62.1 J

60.

53 3\
552/
28.8

54
28.

48. 5 \
48.2/
42.31
42 /

48.

42-

17 9\
17.1/

"7

49 5 \
55 1
4441
44.6/

52
44-

27.5-1
3« /

29

The amount of acetylene absorbed increa.ses under pressure
approximately according to Henry's Law, so the above laboratory
results can be used to predict pretty closely what will be absorbed
under the pressure used in tiie acetylene storage industry.

Part III.— LARGE .SCALE EXPERIMENTS.

In this series acetaldehyde of between 99 and 99.5° purity
was used as the solvent in a regular 6" x 20" acetylene storage
tank, such as are commonly used on autoiuobiles. in order to make
comparisons with solvents in industrial use as to the amount of
gas absorbed, the candle power of the light given on burning the

ACETYLENE SOLVENTS 139

gas from the tank, the loss of solvent, etc. The other solvents were
C. P. Acetone, and a complex mixture of organic liquids, which
is used as a solvent for acetylene, and which will be referred to in
the accompanying curves as Ester-Ketone-Aldehyde solvent, since
it undoubtedly owes its absorbent power to the presence of bodies
belonging to these three groups.

Probably the most important point of comparison is brought
out in the curve for each solvent where the candle power at
various times of the discharge is shown; a striking difference
between the volatile and the non-volatile solvents appears here. With
the non-volatile solvents there is little more than an hour's warning
before the gas is gone completely, while with the volatile acetalde-
hyde solvent there is an interval of from 4 to 6 hours in
length from the first warning and the "going out" of the light.
With the acetaldehyde, there is a round black spot in the flame
that makes its appearance at about the 35 candle power point on
the curve, and the size of this spot increases as the candle power
drops, its appearance giving about 6 hours warning, where two yi
cu. ft. burners are being used.

The loss of solvent, which runs with the non-volatile solvents
is common practice from 4 to 6 ozs. for each discharge of the tank,
was a fraction over 12 ozs. in the acetaldehyde experiment, where
the evolution of the gas was pushed to the lirrtit, and would
undoubtedly run about 8 ozs. in industrial use.

At first glance it appears rather surprising that the drop in
candle power with the increase of solvent vapor in the gas. is not
greater. For example, it is seen from the curve where candle power
is plotted against per cent of solvent vapor in the gas, that
when the solvent vapor has increased to 80 per cent,
the candle power is still above 20. It has been noted by
other observers that diluents lower the candle power of acetylene
more rapidly the lower the flame temperature of the diluent. Since
acetylene has a heat of 313.8 cals. per gram molecule, and acetalde-
hyde has 279.2, we have a satisfactory explanation of the action
of the diluent in this case; the calculated temperature of the hottest
part of the oxy-acetylene flame is in the neighborhood of 4000° C.
and that of the oxy-acetaldehyde flame is above 3400° C.

The aldehyde vapor is a good diluent also for the reason that
the volume of air or of oxygen required for its combustion

140

AMERlC.iy IXSTITUTE OF CHEMfCAL EXGIXEERS

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ACETYLENE SOLVENTS

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146 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

is theoretically exactly the same as that required for acetylene, so
that there is scarcely any change in the shape of the flame, as the
percentage of aldehyde vapor increases.

These two facts, the high heat of combustion, and the equality
of the volumes of air or of oxygen needed make for an advantage
in the use of acetaldehyde as a solvent for acetylene to be used
in welding and cutting operations. In an emergency repair job in
a remote locality, in case the gas gives out the work can be finished
by drawing on the volatile solvent for the combustible.

Long observation has shown that the figures attained in industrial
practice with the non-volatile solvents noted above average 37
ozs. acetylene in 85 ozs. solvent, at a temperature of 70° F. and a
pressure of 250 lbs. gauge. In this experiment with acetaldehyde
as the solvent, 48 ozs. of acetylene was absorbed in 82 ozs. of
solvent, with the gauge standing at 265 when the temperature rose
to 70° F. This figure shows that acetaldehyde is a liquid that has
a superior absorbent power for acetylene, in fact the author
ventures the statement that this experiment shows an amount of
acetylene greater than has ever before been stored in a given volume
of solvent.

Conclusions.

The rapidly advancing price of acetone and other solvents makes
it desirable to have commercially available a solvent that can be
obtained in any quantity and which shall not advance in price
abnormally.

Acetaldehyde as can be seen from the foregoing experiments,
fulfills the industrial requirements ; its volatility can actually be
turned to advantage, as noted above-
Since acetaldehyde can be made in one chemical operation
directly from denatured alcohol, we have here a source of supply
of an acetylene solvent which will not increase in price, but which
will undoubtedly become cheaper as improved methods of agri-
culture make it possible to produce denatured alcohol cheaper.

Acknowledgment.
I wish to state that I am indebted to my former student
assistants, Messrs. E. P. Poste and E. W. Gardner for their help
in taking readings and making records in the above experiments. In

ACETYLENE SOLVENTS 147

this connection, I wish to express my thanks to Dr. H. S. Hower
of the Physics Department, Carnegie Institute of Technology, for
assistance in taking the candle power readings and for the loan
and standardization of the Brodhun Portable Photometer, which
was used in the photometric part of the work.
Chemical Department,

Carnegie Institute of Technology.
December, 1912.

DISCUSSION.

President: Gentlemen, this is a very suggestive paper, because
it has a direct bearing upon the important subject of storing and
using acetylene generally. \'ot only for purposes of illumination,
but also for acetylene welding. When I was a university student I
remember very well that acetaldehyde was cited in research work
as one of the expensive luxuries. It was sold then for something
like a hundred dollars a kilo, but before I graduated, some German
alcohol manufacturers by their methods of distillation began to
produce aldehyde as a by-product and soon it was possible to buy
aldehyde for a few marks a kilo. It is possible that these gentlemen
are able to produce acetaldehyde in large quantities, and that it will
become a real commercial commodity, so that the use of acetaldehyde
will develop ; it is the same old story again, to bring a commodity
in, supply it, and right away it may develop that if acetaldehyde
is thrown into the market for acetylene that they may use it
for a lot of other purposes, and I understand that attempts arj
being made to utiHze it as a solvent. It seems to be destined to
become a competitor of acetone. Acetone has been increasing in
price all the time, and is, after all, a by-product of wood distil-
lation ; it is therefore of limited production, unless those fermenta-
tion methods of production which lately have been announced
in England and France give us a cheaper supply of acetone, but
we have not heard much since that first announcement, which was
made about three months ago.

The subject is now open for discussion.

Prof. Bain : I have learned a lesson to-night in a very curious
way. I walked into the laboratory of one of my colleagues last
winter and this gentleman is very much interested in organic

148 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

chemistry and is devoting all his time and attention to it, and I
cannot say that my ideas run in the same direction. When I
walked in and saw him pouring sgmething into a large flask I
asked him what it was, and he said he was testing the action of
acetylene on acetone. 1 asked him how that came about, and he
said he had been consulted by an agent who was compressing
acetylene in the cylinders for the railway companies, and he got
interested in it, and he warmed up to the subject and told me a
whole lot about it, but, much to my sorrow, I have to say that I
turned a rather deaf ear to it. That man knew what he was
talking about, and now I am trying to think what he told me. He
told me, as far as I can remember, that there is formed a series of
compounds by the action of acetylene on the compound, and the
only substance I can remember is that phorone is one of the
compounds formed there, and there are a number of others. I
am under the impression that he has never published the results,
out I know he spent a good deal of time on it, and no doubt before
very long he will be able to know exactly what compounds . are
formed in its reaction.

Dr. Ittner: I would like to ask if Mr. James has made
experiments on the stability of acetaldehyde itself, whether it
changes readily or not, or whether it is sufficiently stable. Of
course acetone is under ordinary conditions a very stabje compound,
but acetaldehyde — does it answer the same qualifications and is it
stable ?

Prof. James: No, it is not as stable, and one thing we have
to avoid in its use is the presence of alkalis, or the presence of
acids. It is necessary to be very careful about the containers. They
are filled with a porous filling, and in the old method of preparing
that filling, sodium silicate was used, and we have to avoid that.
In answer to Dr. Bain. I venture to suggest that his friend is
mistaken. The acetylene can be all driven out of any solvent by
boiling. My opinion is that this is a chemical action, and the
formation of some compound which decomposes as soon as the
pressure is released.

Prof. B.MN : I simply said that it was my neglect and I paid
no attention to it at the time, so I will not be able to offer you
any information except that simple statement.

President: There is one possibility about acetaldehyde. Its

ACETYLENE SOLVENTS 149

tendency to produce acetic acid by oxidation. Of course it is
only possible in the presence of air. If your acetylene contains
air and you compress it, it will produce acetic acid in the steel
containers.

Member: I think Prof. James is to be congratulated. One of
our fellow members in this country has started on a large scale in
making acetaldehyde.

Member: May I ask if acetaldehyde is on the market now?

Prof. James: No, it is not. We sent out samples to find out
if there should be a demand for it in other lines. We propose
to use it entirely for this industry (acetylene storage) and incident-
ally, if we find a field outside we will make more of it. Of course
we would have to ship it in the form of 50 per cent solution in
methyl alcohol. It is a pretty good solvent, about as good as amy!
acetate, for the nitrocelluloses for example, and we hope to
introduce it for that purpose, but we have not as yet.

Member: It might be interesting to remark that a proposal
has been taken for the use of butylidine glycol instead of glycerine.
It is calculated that if the price of glycerine should become about
24 cents a pound, that butylidine glycol would do for a substitute in
explosive manufacture.

THE NEW CHEMICAL ENGINEERING COURSE
AND LABORATORIES AT COLUMBIA UNI-
VERSITY

By M. C. WHITAKER.

Read at the Detroit Meeting December 6, 1912.

Course of Instruction.

Improved training in Chemical Engineering is a problem which
has received much consideration from this Institute. The
Committee on Education has done valuable work in collecting data
and ojMnions from leading chemical engineers and has offered
many helpful suggestions on this important subject. While no
specific curriculum has been officially adoiited and no definite system
of laboratory equipment or training has been agreed upon, it is
felt that certain points stand out with sufficient prominence to
justify action, and it is upon this basis that we have gone ahead
and initiated the work as here outlined.

The burden of the rapid advance in all engineering science has
been felt more keenly by the student than by anyone else. The
amount of ground to be covered between high school graduation
and the engineering diploma has increased year by year, but the
time allotted for the work has remained the same, — four years.
When the student's "elastic limit" is reached it becomes necessary
to curtail at some point. In some of the schools cultural subjects
are being eliminated from the curriculum to the great loss of the
student's general scholarship ; in other institutions fundamentals
are superficialized to such an extent that the graduate lacks the
necessary foundation on which to develop; in still other engineering
courses, cultural and fundamental subjects are retained and the
engineering applications are given absent treatment. In a few
cases, where the faculty is about evenly divided between cultural
and engineering representatives, the student's wail concerning the

150

.CHEMICAL ENGINEERING COURSE AT COLUMBIA 151

amount of time at his disposal for study, and the assimilation of
the various and varied subjects ofTered in the distended curriculum,
has been drowned by the rhetorical scramble for more time for
each of the "most important subjects" in the course.

The obvious remedy to meet this deplorable situation and to
provide for the rapidly advancing demands of technical education
is to give the student more time to do the increased amount of work.

The engineering departments of Columbia University will become,
in 1914, regular post-graduate professional schools and require
a college degree or equivalent training for admission. It has been
noted for several years that over 20 per cent of the students in
our engineering departments possessed the college degree at
entrance.

The college training taken as a preliminary preparation to this
post-graduate course in engineering must necessarily include the
fundamental mathematics, physics and chemistry, in addition to
the usual college courses. In a carefully arranged curriculum
this ground may be covered in three years. I submit herewith the
course planned by the faculty of Columbia College to meet the
requirements for admission to the new post-graduate engineering
schools. The subjects treated in this undergraduate course are
now to be found in the schedules of practically all colleges and by
judicious elections, the required fundamentals may be satisfactorily
completed in any good institution.

A THREE YEAR COURSE OFFERED BY COLUMBIA COLLEGE TO

FULFILL REQUIREMENTS FOR ENTR.'USTCE TO POST-GRADUATE
ENGINEERING SCHOOLS.

FIRST YEAR

FIRST HALF SECOND HALF

Advanced .-Mgebra (Math, i) 2 .-Vnalytical Geometry (Math. 4) 3

Chemistr>', Gen'l (2 Lect.) (Chem. Chemistry, Gen'l (2 Lect.) (Chem.

3C.)(6Lab.) 5 4c.) (6Lab.) 5

English Composition (Engl. A) 3 English Composition (Engl. A) 3

Principles of Science; Principles of Science:

(Philosophy .\) 3 (Philosophy A) 3

Modem Language based on Interme- Modem Language: (continued) 3

diate Entr. requirement 3 Shop Work (i Mt.) i

Shop Work (i Aft.) i Physical Education A i

Physical Education A i — •

Total Points 37

152

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

SECOND YEAR

FIRST HALF

SECOND HALF

Calculus (Math. 15) 3

Chemistry (Chem. 67) (2 Lect.) Qual-
itative (6 I,ab.) S

Introduction to Eng. Lit.:

(English B 3) 3

Epochs of History (Hist. A) 3

Drafting (2 afternoons) 2

Geometry:

Descriptive (Drafting 3) 3

Calculus (Math. 16) 3

Chemistry (Chem. 68) (2 Lect.) Qual-
itative (0 Lab.) 5

Physics (3 Lect., 3 Rcc.) 6

Epochs of History (Hist. A) 3

Drafting (2 afternoons) 2

Total points 38

THIRD YEAR

SECOND HALF

Calculus (Math. 17) 3

Physics (3 Lect.,) (3 Rec. i afternoon

Lab.) 7j

Political Science (Econ. 1) 3

Mineralogy (2 Lect.) (1 afternoon) 3

Calculus 3

Physics (same) 7J

Statics (Mechanics 2) 3

Political Science (Politics 4) 3

Surveying (Civil Eng. 2) 2

Total points 35

To make up the re(|uirement of 124 j)oints for the degree of
B. S., 14 additional points must be made either by extra credit
for high standing, by work in Summer Sessions or by free election
during the second and third year of the program; such election
may be made at the student's option from among the courses in
which he can satisfy the prerequisites, with the single provision
that no program aggregating more than 22J/2 points will be approved
for any half-year.

NEW THREE YEAR POST-GRADU.\TE COURSE IN CHEMICAL
ENGINEERING.

FIRST YEAR

FIRST HALF

Subjeci Jlrs.

Physical Laboratory o

Mechanics 3

Industrial Chemistry 3

Power Mahrinery 2

Physical Chemistry 3

Elements of Electrical Engineer-
ing 2

Hydraulics — Theory 2

Quantitative Analysis 2

SECOND HALF

Subject Hti. Aft.

Advanced Heat 3 o

Mechanics 3 o

Industrial Chemistrj' 3 o

Power Machinery 2 o

Physical Chemistry 3 i

Electrical Machinery 2 o

Hydraulics — Laborator>' o i

Quantitative and Engineeimg

Chemistry 2 3

Total 17

Total 18

CHEMICAL ENGINEERING COURSE AT COLUMBIA 153

SUMMER WORK.

CHEMICAL FACTORY INSPECTION (2 weeks)

Factory Work and Detailed Report on Some Assigned Industry (6 Weeks)

second year

first half second HALF

Subject Mrs. A/I. Subject Hrs. Aft.

Organic Chemistry 3 2 Organic Chemistry 3 2

Machine Elements 2 o Machine Elements 2 o

Food and Sanitary Chemistry . . 3 o Adv. Industrial Chemistry 3 o

Engineering Thermodynamics. .3 o Engineering Thermodynamics. .5 o

Direct Current Laboratory i i .Alternating Current Lab i i

Resistance of Materials 5 2 Assaying 2 2

Total 17 5 Total 16 s

SUMMER WORK.

CHEMICAL AND MECHANICAL ENGINEERING LABORATORY (8 weeks)

THIRD YEAR

FIRST HALF SECOND HALF

Subject Hrs. .Aft. Subject. Hrs. Afl.

Introduction to Metallurgy and Metallurgy — Lead, Zinc. Gold,

Metallurgy of Copper 3 o and Silver 3 o

Metallurgy — Iron and Steel i o Chemical Factory Management . 3 o

Chemical Factory Machinery ... 3 o Steam Power 4 2

Electrochemistry 2 i Business Law 2 o

Gas Power 2 i Chemical Engineering Lab. :

Commercial Organic .Analysis ... 2 3 Special Problems o 3

Seminar 5 o Seminar '. 6 o

Total iS 5 Total 18 5

Corresponding courses have been adopted for Alining, Civil,
Electrical and Mechanical Engineering and it is believed that this
extension of practically two years in the amount of time to be
devoted to the fundamental and professional work together, will
not only relieve the present tension on instructors and students,
but will produce a class of graduates immeasurably better qualified
to assume the responsibilities of their profession.

Chemical Engineering Laboratory.

Chemical Engineering courses must eventually teach men to
use engineering methods and engineering appliances in the solution
of chemical problems and the operation of chemical processes.
These engineering methods and appliances are not to be found

154 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

in the test tube, beaker, or funnel of the chemical laboratory any
more than steam engines, hydraulic machinery, electric generators,
and switch boards are to be found in a physics laboratory.
Mechanical and electrical engineers long since saw the difTerence
between the equipment needed for studying the application of the
fundamental scientific principles to complicated engineering con-
ditions, and the equipment to be used to study the laws and
principles upon which these fundamentals are based, and accord-
ingly established laboratories equipped with mechanical and elec-
trical engineering apjiliances to meet these needs.

The chemist, on the other hand, with the characteristic conserva-
tism produced by many disappointments, is slow to recognize the
point at which the study of principles ends and the study of
a])plications begins. He hesitates to develop laboratories with tanks,
sii>hons. pumps, filter presses, evaporators, stills, centrifugals,
absorption towers, etc., but prefers to consider his work complete
with the establishment of a principle on a test tube scale. The
chemical engineer is sorely needed at this point to take chemical
principles and engineer them just as the mechanical engineer
engineers the physics of heat, or the electrical engineer engineers
the physics of electricity. The chemical engineer has small chance
of engineering chemical operations unless he knows the fundamental
methods and appliances available. He cannot establish data with a
beaker and a test tube on which to engineer a process any more than
a mechanical engineer can arrive at a correct conclusion in regard
to the performance of a steam boiler by some experiments with a
tomato can.

It seems clear to me therefore that our students must study
the methods, appliances and engineering principles involved in
chemical operations by contact with the equipment developed for
this field. Furthermore, our researches, where industrial applica-
tion is sought, must be transferred from the beaker to the tank,
from the funnel to the filter press, from the evaporating dish to
the vacuum pan. from the distilling flask to the still, and so on.
before any data on which to base judgment as to it.s practicability
can ever be established.

I am establishing at Columbia, with the support of Dean Goetze
and an administration which seems to have the courage of my
convictions, a chemical engineering laboratory in accordance with

CHEMICAL ENGINEERING COURSE AT COLUMBIA

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156 AMERICAX ISSTITVTE OF CHEMICAL ENGISEERS

CHEMICAL EXGIXEERIXG COURSE AT COLUMBIA

157

the plan outlined. The accommodations are by no means ideal
and the scheme is far from complete, but we have made a bold

Fig. 3. — Double Effect Vacuum Pans.

beginning. We hope to expand rapidly from year to year and
ultimately have a laboratory of chemical engineering comparable
with the best laboratories in mechanical and electrical engineering.

158

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

Some photographs will serve to show the plan and scope of
our work and the progress thus far made. The chemical engineer-

FiG. 4. — Column Still anJ Extractor.

ing laboratories and the electrochemical laboratories occupy the
entire lower floors of the 1 lavemeyer Building. The division of
space is shown by reference to Fig. i . from which it will be noted

CHEMICAL ENGINEERING COURSE AT COLUMBIA 159

that we have, besides the large general laboratory, the electro-
chemical laboratory, paper and textile laboratory, research labora-
tories, grinder room, pipe shop, machine shop, etc. Some of the

Fig. 5. — Shelf Drier and Vacuum Pumps.

more typical equipment now installed and in operation will be
illustrated by reference to Figs. 2 to 7.

The Chemical Engineering students use this apparatus not

160 AMERJCA.X ISSTITVTE OF CHEMICAL EyChXEERS

CHEMICAL ENGINEERING COURSE AT COLUMBIA 161

162 AM ERIC A\ ISSTITUTE OF CHEMICAL ENGI SEERS

only as types of efjuipment already developed to carry out the
desired operations, but they soon become familiar with the limita-
tions of the appliances and have to exercise engineering judgment
in overcoming the difficulties. The research men lind standard
e(|uipment of modern and approved type ready and available for
trying out any fundamental practice on a scale and in a way which
will enable them to establish data capable of being used in
business calculations or works engineering. The problems arising
as a result of transferring operations from the laboratory to the
large scale factory appliance may here be met and solved under
the sympathetic eye and patient hand of the developer, instead of
being doomed to failure by being delivered in incomplete form to
unsympathetic and busy works managers.

The problems assigned in all of these operations have been
selected so as to be cyclic, and thus avoid production operations.
For example, in the work involving the use of the tanks, siphons,
pumps, tiller presses, etc., a s(|uad of four or live students begins
by dissolving a weighed quantity of the waste sulphates of the
didymium earths in dilute sulphuric acid in a lead lined tank with
air agitation. This solution is transferred with a lead siphon and
precipitated as an oxalate, the licjuid returned to the lead tank for
future use, the precipitate washed by decantation, filter-pressed, the
press cake transferred to an iron tank and converted to hydro.x-
ides. The soluble oxalate is stored for use in the evaporator
and the hydroxides are dissolved in acid and returned to the
first tank. During these operations, the student has had experi-
ence with solution, precipitation, washing by decantation, filtration
of a granular crystalline precipitate, conversion from a solid
insoluble in acid to one soluble, filtration of a slime and resolution
in acid, air, steam and mechanical agitation, pumps, siphons, etc.
All of this work is done on a quantitative basis and losses are
checked and accounted for at each stage of the work.

Similar cyclic operations have been devised for all of the
units of the laboratory with the object of reducing operating
expenses to a minimum and also avoiding the accumulation of a
product. Students are given the greatest possible liberty in the
methods of handling their problem, are allowed to make mistakes
and get experience. The instructors are there to assign problems
and supervise the work, but not to dictate and direct.

' CHEMICAL ENGINEERING COURSE AT COLUMBIA 163

DISCUSSION.

Member: I would like to ask Prof. Whitaker in just which
course on this schedule the students utilize this equipment.

Prof. Whitaker: It must be apparent that such a laboratory
course as this could not be successfully given unless you had a
considerable number of consecutive hours, and I propose, there-
fore, that the major portion of this work be given in the summer,
so that I can get the boys in at 7 in the morning and keep them
until 6 at night, if necessary for eight weeks.

Prof. Smith : I am delighted to know that some institution
has taken up the teaching of chemical engineering in this way. It
has been my idea for years that it is the right way to teach the
final steps in the engineering student's education. I have had some
such course in metallurgy as this, at Case School, for a number of
years, and I have found one important item of advantage already in
it that Prof. Whitaker did not mention. I added a blast furnace.
I know Columbia University does not believe in their metallurgy
department having students operate a blast furnace, but I do not
believe it bad to teach them the operation of it, and I do think
they get in that operation a great deal of enthusiasm for their
work. They think they are doing something, and they go back
to their lectures with new ideas, which is very satisfactory to
their instructor. The plan of giving students knowledge of these
fundamental principles is most valuable; if they do not have this
when they go into the work, the workmen, foremen and everybody
connected with the place have a contempt for the college man, and
he must stay there three or four years before he can live down
that handicap that he gets the first few years of his employment
in the factory. If he can give the idea that he knows either how
to put together a lot of pipe, or lace a belt and put it on to a
pulley, and a few fundamental things of that kind, the workmen
there think that he knows something. They think if he cannot
do that he is absolutely no good, and if he can do that he gets
their permanent respect at once.

Secretary Olsen : I would like to ask Mr. Whitaker if this work
comes during the summer following the fifth year?

Prof. Whitaker: Yes.

Secretary Olsen : I would like to point out in this connection

164 AMERICAN INSTITUTE OF CUEKtlCAL ENGINEERS

that in this course, the student who undertakes this work has had
one year more of college work than is ordinarily undertaken at
present, when the student goes into a business. That is, having
finished five years of college instruction, he will have had more
instruction in chemistry, and other sciences, than he would have
had after the ordinary four years' course. This chemical engineer-
ing laboratory has introduced the idea that instead of the student
going into the factory and making his breaks there, he will get his
experience under the supervision of tlie college professor in that
eight weeks' summer time, and he is better fitted for doing it by his
college instruction, and goes into a laboratory equipped for him
to study the factory operations.

I want to make this remark in addition. It seems to me it is
a splendid idea. I think it marks an advance in chemical engineer-
ing instruction which, it seems to me, is of the greatest importance.
I notice that the student will have had two weeks of factory inspec-
tion at the end of his fourth year. I also notice that in his fifth
year he remains in college after he has had his summer of factory
■ inspection. After he has had his summer work in this chemical
engineering laboratory, he is then to have a sixth year of college
instruction, and his college professors are going to have an
opportunity of showing the relation between this and the factory,
to point out the important steps and the relation between practice
and science. So it seems to me after he has finished that sixth
year he ought to be able to go out and be far more successful than
any graduates that we have at present.

Prof. J.xMEs: I think Dr. Whitaker is doing a great deal of
good in this pioneer work. He is working right along the lines
of some dreams I have had in teaching students the fundamental
operations of chemical engineering. We expect to do that in our
institution as soon as we get money enough. I believe that for
one to understand these fundamental operations is to a certain
extent to insure that he will make a success the first year he is
out of school. In other words, he will make good right away.
I think he has a great deal better chance for success. That is one
of the things that will result from work, in this course of chemical
engineering. Another thing is that it is an opening wedge for
research w'ork in chemical engineering, as such. When the insti-
tutions of the country that can afTord it will liave such equipment

CHEMICAL ENGINEERING COURSE AT COLUMBIA 165

as that we will have research work that is greatly needed, perhaps
large scale work that no one firm undertakes. I believe that various
institutions will follow Prof. Whitaker's example, and I propose
to follow it in my own place; that is one of the good results from
his work.

Prof. WiTHROW : I want to congratulate Prof. Whitaker on
the progress he has made in this direction, and also to emphasize
it as my own firm belief that this is in the right direction. I also
want to especially commend what most of us who have had experi-
ence in teaching industrial chemistry have learned, and that is
the importance of letting students learn by error. I think we,
ourselves, learn more in consequence of the mistakes we have made
than in any other way. I think it is extremely important at this
stage that the student should learn these things.

Prof. White: I think it is perfectly true that "nothing
succeeds like success," and I have not the slightest doubt but that
under Prof. Whitaker's direction this laboratory at Columbia
University will produce noteworthy results. I am glad to have had
Prof. Olsen emphasize the fact that this was a five year course
and in general this method is not applicable to a four year course.
I desire to question, also, whether it is not possible to do some of
the things Prof. Whitaker emphasizes, without actually resorting
to laboratory work. It does not seem to me absolutely necessary
that a man should have to wait until he tries to produce a solution
of aluminium sulphate in water to realize that on the technical
scale you have to consider what your curve solubility is. By the
time you study on a technical scale the manufacture of aluminium
chloride, etc., you ought to learn that the whole system is based
upon the knowledge of solubility curves in the same way as other
salts. There a man will undoubtedly remember, after he has made
a fool of himself, that he ought to have known, and it is a good
thing to have as many mistakes behind you as possible before you
go out into the world, where mistakes are very expensive, but it
does not seem to me that for a four year college course a laboratory
of this sort is necessary. I admit, it is a fine thing where a person
is studying the multiple efifects to be able to get down and see
the nicety of it, and the layout of it, but the fear that I have for
a laboratory of this sort is that if it is introduced in our colleges
with a four year course the student will become so absorbed with

166 AMERICAN IXSTITUTE OF CHEMICAL ENGINEERS

the machine tliat he will forget the work. In other words, I am
afraid that unless it is managed very carefully it would degenerate
somewhat into a kindergarten work. As a graduate department,
I think it is splendid. I wish we could have one here, but I
have no ambition to duplicate that plan in our four year students'
course.

Dr. Arthur C. Langmlir: I think Dr. Whitaker is not only
working exactly in the right direction but I wish he had 5 to 10
millions at his disposal, because I should like to see a laboratory
equipped with not only evaporators, showing their practical effects,
and centrifugal machines, etc., but the very best and latest types
of machines on the market. I should like to see such an institution
be able to afford the luxury of a scrap pile and scrap things if
they became the least antiquated. It seems to me such an institu-
tion could lead the chemical industries, and be far in advance of
many lines of chemical industry, and the students they send out
in a majoritj' of the cases would be able to be of some advantage
to their employers and undoubtedly be able to point out many
ways in which they could better their equipment and economize.
I think that we will live to see such an institution before many
years. I think that Dr. W'hitaker is to be congratulated on having
made the start that he has.

In regard to teaching the principles of the subject it does not
seem to be wrong or impracticable to teach a man, for instance,
the principles of evaporation by means of quadruple effect and
interchange of heat. I do not see why we cannot understand the
principles to better advantage there than he can with fuel and a
barrel full of water. Such etjilipment is not so good.

President B.\ekel.\nd: Prof. Whitaker in his usual modest
way forgot to point out the most important piece of apparatus
which is necessary to make a success of the equipment he recom-
mends. We can easily purchase triple effect vacuum plants and
any other machinery ; any such equipment is not very expensive
and will cost only ten, twenty or thirty thousand dollars. But the
most important, the most indispensable part of the whole equip-
ment is the teacher himself, and he cannot be obtained as readily
as any piece of machinery, however expensive the latter may be.
But it so happens that by sheer good luck, Columbia University
has acquired a man who has earned his spurs in the industry, after

CHEMICAL ENGINEERING COURSE AT COLUMBIA 167

having been a teacher, and then was wilHng to drop his well paid
position in an industrial enterprise, and work for a small salary
for the good of his University, and of chemical education. This
kind of "apparatus," for a chemical engineering course, a first class
technologist, who is at the same time a good teacher, I fear very
few universities will be able to purchase, as long as the induce-
ments which are offered nowadays by our educational institutions
are so small. I refer less to the slender salaries, which are paid
to professors, than to the irksome feeling of a man of individual-
istic tendencies of submitting himself slavishly to the dictates of
some Board of Trustees, made up of men whose mental qualifica-
tions are frequently subordinated to the fact that they are giving
financial support to the institution. Such conditions frequently are
more discouraging than a small salary.

I believe that an extended course like the one outlined by
Prof. Whitaker, may, in the end, prove a gain of time to the
student. Anybody who employs a young chemist knows what a
job he has to get him through the first year of his employment
and to turn him to some use. The young chemical engineer who
knows it all, seldom earns his first year's salary, however small,
although he frequently earns the contempt, if not the hostility, of
every workman in the factory. The initial salary you pay him
serves merely to find out whether there is some hope that,
ultimately, he may be trained to amount to something. I would
call it a "prospecting" investment. An extra year for a man
taking Professor Whitaker's course would therefore seem a good
investment for the student in chemistry. In his curriculum he will
have encountered those elementary practical problems which occur
in almost every chemical industry, and he will be better prepared
to cope with them in practical life. The standpoint of Professor
Whitaker seems too self-evident to need any defense whatever.
Long ago, it was adopted by all other engineering professions.
Why should it be different for chemical engineering?

I would like to point out to Prof. Whitaker that as far as my
personal experience goes, some of the lectures which have done me
most good in my connection with the business side of chemistry,
were some lectures on political economy, which I followed when I
was a beginning student. I think political economy is almost indis-
pensable in a curriculum of chemical engineering, but probably Prof.

1G8 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

Whitaker has good reasons for not mentioning it. I desire however,
to formulate a general criticism against any curriculum which
extends over too many years ; it kills the initiative and the spon-
taneous judgment of the better class of students; only the more
passive or less alive students have the patience to stand long years
of preparation before jumping into the harness of practical life, and
personal responsibilities, where they can better sharpen their wits
and test their abilities than by mere book-wisdom ladled out in
school after cut and dried pedagogic rules. School education ought
simply to provide the means and the enthusiasm for further intense
self -education.

Prof. Whitaker: I believe one of the greatest difficulties in
getting the support for these chemical engineering laboratories is the
chemists themselves. It seems to be so utterly impossible for them
to agree upon what should and what should not be done. One is
afraid to ask the support of people who have means, for fear they
will consult some other chemist, where the chances -are about even
that the other chemist will tell the capitalist that you are crazy.
I cannot help but think that whatever we do we might agree and
concert our actions on this problem. As far as the cost of this
work goes, I have figured a number of times, and think I have
stated that one-tenth of one per cent of the net profits of the
chemical industries of this country for one year would build and
equip one of these laboratories, and that that amounts to more
money than is now invested in the chemical engineering laboratories
of America and Europe put together. Such a situation as that does
not exist in any other engineering subject. I would submit that
when you hire a mechanical engineer you can get him in the boiler
house without blindfolding him. but when you hire a chemical
engineer many have not seen a filter press and do not know where
the slimes go in and where the filtrate comes out. If this scheme
of education has come to stay and is filling the bill for these
other engineering subjects, how can we avoid the final issue in
chemical engineering?

Prof. W'lTiiRow: Each one who teaches Industrial Chemistry or
Chemical Engineering is naturally guided by his own practical expe-
rience in emphasizing or molding his course. For the last six years
it has been impossible for me to secure in my own work at Ohio
State University any adequate apparatus. I have not been entirely

CHEMICAL ENGINEERING COURSE AT COLUMBIA 169

discouraged by this feature, however, because many years before ever
starting to teach the subject I had formed certain notions as to the
importance of the proper point of view toward manufacturing
problems as a result of my personal observation in the works, and
consequently in my work here these ideas are emphasized very
strongly without the use of much apparatus. ^ly point of view
has been to emphasize especially the feature that the problems of
the factory are to be solved by the research spirit, and I have there-
fore made my own course entirely industrial chemical research.
This has given me an opportunity of incorporating a great many of
the ideas which have been mentioned in this paper and in the dis-
cussion. However, I must say that I sincerely feel the lack of
chemical engineering equipment and as soon as it is possible to
secure the same, I intend to utilize it, for I believe it has much value.
To Professor Whitaker, therefore, belongs the credit for having
been the pioneer in securing and emphasizing the importance of
such equipment, especially showing the way to the fact that equip-
ment can be obtained if we go after it properly.

Upon examining the new course as proposed at Columbia
University, I do not agree with a former speaker that this course
of Professor Whitaker's is necessarily a graduate course, for, while
it is true that it comes between the fifth and sixth years, it will also
be noticed that it comes only at the end of or in cortjunction with
the fourth year of Chemistry because no chemistry at all is contem-
plated in this course during the first year. I would, therefore, like
to ask Professor Whitaker a question — "If Columbia University
had not gone on the six year basis, would he not have endeavored
to find room for such work as he has described in or connected with
the old four year course?"'

Prof. Whitaker: Such a laboratory has a double function, first
as a basis for instructing undergraduates in the methods of the Engi-
neering of Chemistry, and second as a laboratory where research
in Chemical Engineering may be conducted. We would undoubtedly
have established such a laboratory and used it for both purposes.

THE NEED OF STANDARD SPECIFICATIONS IN
OILS FOR PAVING BLOCK IMPREGNATION

BT JOHN HAYES CAMPBELL

Read at the Detroit Meeting, December 6, igi2.

Tlic increasing use of impregnated blocks for street paving
consumes larger quantities of creosote oil each year. These oils
are supplied under specifications which prescribe definite specific
gravities, fractions on distillation and insoluble matter, but
unfortunately the mode of stating these constitutents varies greatly.

It. is with a view of bettering this condition, and to suggest
a Committee, to adopt a standard specification, that the data in
this paper has been gathered.

The Wood Preservers' Association and the American Rail-
way Engineering Association have formulated a method of
fractionating creosote oils for tic and timber impregnation, and
if tlie Institute of Chemical Engineers do the same for the paving
block oils, the creosote oil industry would be well covered.

The Railway Engineering Association Specifications are as
follows :

The oil used shall be the best obtainable grade of coal tar
creosote ; that is, it shall be a pure product obtained from coal
gai tar or coke oven tar, and shall be free from any tar, oil or
residue obtained from petroleum or any other source, including
coal gas tar or coke oven tar; it shall be completely licjuid at 38°
C, and shall be free from suspended matter; the specific gravity of
the oil at 38° C, shall be at least 1.03, when distilled by the common
method ; that is. using an 8 oz. retort, asbestos covered, with
standard thermometer bulb Y> inch above the surface of the
oil — the creosote, calculated on the basis of the dry oil shall give
no distillate below 200° C, not more than 5 per cent below 210°
C, not more than 25 per cent below 235° C, and the residue
above 355° C, if it exceeds 5 per cent in (juantity, shall be soft.
The oil shall not contain more than 3 per cent water.

170

SPECIFICATIONS IN OILS FOR PAVING BLOCK IMPREGNATION 171

In addition to tliis standard grade, two inferior grades can be
used in cases where the higher grade oil cannot be procured.
As the second and third grades differ only in specific gravity
and fractionation, the wording of the specification being the same
as quoted above, I will simply indicate them to save space.

No. 2 grade specific gravity at least 1.03 at 38° C, liquid
at 38° C. Fractionation: below 210° C, not more than 8 per
cent, below 235° C, not more than 35 per cent, if residue above
355° C. exceed 5 per cent, it must be soft. Not more than 3 per
cent water.

No. 3 grade. Specific gravity at least 1.02 at 38° C, completely
liquid at 38^ C. Fractionation: below 210° C, not more than 10
per cent, below 235" C, not more than 40 per cent, and the residue
above 355° C, if it exceed 5 per cent, must be soft. Not more
than 3 per cent water. (Railicay Agc-Gazcttc, Mar. 12, 1912.)

A much quoted specification follows:

Specific gravity at 38° C, at least i.io completely liquid at
25° C, and show no deposit on cooling to 22° C, not more than
3 per cent insoluble by hot continuous extraction with benzol
or chloroform. Fractionation: up to 150° C, nothing must come
off; up to 170° C, o per cent to 5/10 per cent; up to 210° C.
2 per cent to 4 per cent ; up to 235° C, 6 per cent to 16 per
cent and up to 355° C, 40 per cent to 55 per cent. Thermom-
eter to be corrected for emergent stem, not more than 2 per
cent water will be permitted.

Another specification much used by City Engineers is as
follows :

Specific gravity at least 1.03 and not over 1.C9 at 38° C.
Insoluble in benzol and chloroform not to exceed 5 per cent.
Not more than 3 per cent water; if it contains this amount, allow-
ance must be made in treating for w-ater. Fractionation up to
150° C, not to exceed 2 per cent; between 150° C. and 170° C,
not to exceed 15 per cent; between 170° C. and 235° C, not to
exceed 30 per cent ; between 235° C. and 300° C, not to exceed
35 per cent all as dry oil. Residue shall be soft and adhesive.
Shall contain about 25 ])er cent crystallizable naphthalene and at
least 15 per cent anthracene oils.

Thirty-eight degrees C, or 100° F., is by agreement the accepted
temperature for delivery of creosote oil, a variation of temperature

172 .l.Ur.R/CAX IXST/TUTE OF CHEMICAL EXCJNEERS

above or below this point being corrected at i per cent volume for
each 221/2° F. or 12^° C. This would make a variation of
o.ocx)8 specific gravity for each 1° above or below 38° C.
Specific gravities should be so determined and reported.

Insoluble matter is probably best determined by the method
of H. M. Newton (Report Sixth Annual Meeting of the Wood
Preservers' Assn. 1910). Two grams of the oil are weighed into
a small beaker. Twenty volumes of benzol are added and the
mi.xture thoroughly stirred. Two S. and S. No. 589 Blue Ribbon
filter papers and i double thickness S. and S. shell, 80 x 22 mm.
in size and tarred on a balance against two other filter papers and
one shell, the papers and shells having previously dried in a desic-
cator. The tare is returned to the desiccator. The two filters are
folded and one placed within the other, and the diluted sample
filtered through them. The beaker is washed with an amount of
benzol sufficient to transfer all particles to the filter papers. When
the papers have drained, they are rolled up and ])lace(I in a
• Soxhlet extractor, and extracted with the filtrate from the filtra-
tion of the sample, until the solvent runs off colorless. It is then
dried in an oven at about 80 to 90" C, together with the tare, and
when dry is cooled in a desiccator, then weighed. Some of the
original sample is in the meantime, filtered through a double
filter of the same quality as previously used, no weight being
taken of the papers. Two grams of the filtrate are taken, and
subjected to exactly the same procedure as outlined above.
Weight No. i gives weight of suspended matter plus anything
thrown out of the oil under examination by benzol. Weight No.
2 gives the weight of precipitate by benzol only. The per cent
of matter precipitated by benzol as obtained from No. 2 must not
be calculated on the weight of filtered oil taken, but on the amount
of unfiltered oil which would furnish this amount of precipitate,
by the following data and formula :

X = free carbon or insoluble.
11' = weight of unfiltered oil taken.
ir' = weipht of free carbon plus precipitate.
£ = weight of filtered oil taken.
£' = weight of precipitate.

E
^ = £^-.

(looir' ioo£'\
- ir '~~E~)'

SPECIFICATIONS IN OILS FOR PAVING BLOCK IMPREGNATION 173

We now have specifications which have given satisfactory resuhs
in service, and methods for assaying the oils furnished under them ;
and are prepared to go into conditions confronting engineers in
different parts of the country, when they invite tenders on paving
material.

The coast cities can obtain the imported oils, which would
meet all the conditions of the Railway Engineering Association
specifications. The Eastern West, Middle West and West, east of
the Rockies, must depend upon American oils, or mixtures of
American oils with refined or crude tar in various proportions,
and here is where the great cause of friction between inspectors
acting for municipalities and paving block contractors has its
origin. In the Middle West little if any creosote oil free from
added tar is used for paving block impregnation.

The majority of specifications have a clause in them, stating
that a pure coal tar product shall be used for oil, the cut off points
of fractionation are stated and the amount of residue if above
a certain point must be soft. The inspector, if he is at all
conscientious, will balk at accepting that oil which he is reasonably
sure contains added coal tar, without submitting the matter to
the Engineer for whom he is acting. The Engineer has his street
torn up, traffic is interrupted and he writes or wires to accept
that which is positively prohibited by the clause under which the
inspector is working. This places the inspector in a bad position
in future contests. In view of these facts, the following procedure
would avoid these contests. Apply the First Railway Engineer's
Assn. specifications to the imported and American lighter creosote
oils. Then make two other grades. No. 2, to contain a mixture
of 70 per cent American or imported creosote oil and 30 per
cent refined coal or coke oven tar, No. 3 to contain 40 per cent
of American or imported creosote oil and 60 per cent of refined
coal or coke oven tar.

This procedure would permit the Engineer to make the choice,
best suited to his local conditions, and not force him to buy a
spade under the name of a long handled shovel.

Appended are some assays of these various oils.

It will be noted that the straight American oil is below the
first specification, but it was submitted for these tests by a reput-

174

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

Imported Creosote Oil, Average of Five Assays

Specific gravity at 38° C i .056

Suspended or insoluble 0.27%

Up to 200° C 0.91 per cent

" 210° C 3.68 "

" 235° C 23.89 "

" iSS° C 80.87 "

Residue above 355° C 19'i "

Water 1.94 "

Residue pasty

American Creosote Oil. 7o9i Oil, 30% Tar

Spec. grav. at 38° C 0.9901 i .03

Insoluble 0.28 1.22

Water none

Up to 200 1 2 . 04

210. . . .

" 235- •••

" 355---

Residue pasty .

none
II 16
17 70
47 99
93-67

6-33

none

none

6 21

6 51

10. 5S

10.49

29.27

29.76

74 34

74 17

25.66

25.83 Pitchy

60% Oil and 40% Tar
Specific gravity at 38° C ..
Insoluble

40% Oil and 6o9c Tar

1.094

Water none

Up to 200° C 5 . 53

" 210° C 9

" 235° C 25.34

" 355° C 68

Residue 31

none
5 97
9 55
25.62
68.66

none

3.62

78

Done

3-28
5 42
17 56
55 54

31.34 Pitchy 45 23 44 46 Pitchy

Unrefined Tar

Water 2.38

Up to 200° C 7 . 59

" 210° C 9.04

" 235° C 16.92

" 355° C 39 . 62

Residue pitch 60 . 38

Specific gravity at 38° C 1 150

able manufactory with full knowledge that the sample was to be
used for this work and is probably a good, average American oil.

Specifications using the term, if the residue e.xceeds 3 per cent,
it must be soft, should state the temperature at which this residue
should be soft. It would probably be better to say, when kneaded
between the teeth, the sample must be soft and plastic, not crumbly.

Secrkt.vry: The author calls for a resolution or some action of
the In.stitute in connection with the paper.

Mr. Campbell is probably very much interested in this, and

SPECIFICATIONS IN OILS FOR PAVING BLOCK IMPREGNATION 175

we have several other members who are very much interested in
this Hne of work, and who are fully capable of acting on a
committee of this kind, if the Institute should see fit to adopt the
resolution which is suggested, and a committee be appointed to
act with these other associations in this matter.

President : I would like to hear the views of the members
present on this subject.

Dr. Ittner: I do not know as it would be wise to adopt the
specifications, because it seems to me that the people to adopt
specifications are the users of creosote, and those who furnish it.
I think we might recommend that specifications be adopted,
but I do not think it would be wise for us to adopt the specification,
as Mr. Campbell gives them.

Mr. Booth: If it is in order, I move you that the chair
appoint a committee to look this matter over thoroughly, with-
out any question of whether the recommendation shall be adopted
or not adopted.

Dr. Langmuir: Second the motion.

President: The subject is open for discussion. Before opening
the discussion I would like to remark that this looks to me like a
highly specialized subject, and I am not aware that we have many
members here who are sufficiently prepared to pass an authoritative
opinion on this question.

Mr. Booth : In my opinion, the matter should not be settled by
a committee of our members that you might choose. It is not
necessary to settle it here or now.

President: I must confess that I do not know who are the
members who are capable of passing on the subject.

Mr. Booth : The secretary so indicated while he was reading
his paper.

President : Who are the members who are especially so
qualified?

Member: We have Mr. Dow of New York City, and Mr.
DeCew, and I think Dr. Olsen knows a third man.

Secretary Olsen : Dow is a very active man in this line, and
Mr. DeCew, and Dr. Sadtler, and Mr. Peckham.

Dr. Langmuir : We have sufficient talent in our own association,
but nevertheless it does not seem to me that it is the thing we
should take up, but it is a thing for other organizations to take up.

176 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

President: Unless you are entirely convinced that it would be
very useful, this is one of those responsibilities that sve might
just as well try to avoid. If we are going to nominate a
committee, that committee will have to report on the matter, and
the matter will have to come up again, and the committee must
decide, and more than one evening shall have to be taken up to no
purpose. If we undertake the subject we must do it thoroughly or
not at all. Is it worth the trouble and are we qualified?

Dr. Ittner: I read that paper coming in on the train and I
confess that I think it is entirely out of our province to adopt
specifications for a purpose such as he mentions there. I think
it is the province of the civil engineer. I think the chemical
engineers, those of us who are in that line of work, would probably
be best able to recommend such specifications, but I think that it
is out of our province to adopt such specifications and would be a
great mistake for us to go so far as to adopt them.

Mr. Booth : It is not my idea to carry this to a conclusion and
■ adopt such a specification, because I am opposed to it, but we must
show our members courtesy, and that is the only reason I made the
motion, and if the chair so feels I will withdraw the motion. If
there is a better way, let some other member indicate it. I am
absolutely neutral in the matter.

Prkside-vt: So am I. I have no reasons for deciding one
way or the other. I thought it my duty to point out to you the
conditions. There ought to be a sufficient reason for incurring the
trouble and responsibilities which are involved here.

Prof. With row: I have a feeling, too. The idea has been
expressed that we do not want to go into the business of making
specifications, but I wonder about one other point; I was in the
manufacture of creosote oil, and I know those engineers who are
supposed to be the ones who make the specifications make very
ridiculous and impossible specifications, so it occurs to me, that it
might be possible for the manufacturers to suggest something, as to
whether there is or has been a difficult situation. I know when this
industry comes up we will be in touch with it. The specifications
were absolutely worthless to the most important users in the country
at that time.

President : I think a way of settling that question would be to
submit these recommendations to the Bureau of Forestry, where we

SPECIFICATIONS IN OILS FOR PAVING BLOCK IMPREGNATION 177

have to deal with people who are entirely independent of com-
mercial enterprises, while, if we attempt it here there will be only
two or three members of this Institute and every one of them may
be connected with business enterprises.

Mr. Booth : I am perfectly willing to withdraw the motion if
we can show this man proper courtesy.

PRE.SIDENT : I think the fact that we have submitted this matter
to discussion is sufficient courtesy.

THE PRESENCE OF OXYGEN IN PETROLEUMS
AND ASPHALTS

By SAM. P. SADTLEB, Ph.D.

Read at lite Joint Meeting with the Eighth International Congress of Af<l>lied
Chemistry, New York, September 6, 1912.

The problem discussed in this paper may be stated as follows:
Can the presence of oxygen in petroleum and asphalts be estab-
lished by a direct method of ultimate analysis?

To get the full import of this question a few words of intro-
duction are needed, bearing upon the subject of what those inter-
ested in the chemistry of petroleum and asphalt know with regard
to this matter of the presence of oxygen in substances of these two
classes.

Hoefer (Das Erdoel und seine Verwandten, 2 Auf., Seiten 55
and 56) gives a list of 59 ultimate analyses of petroleums from all
countries. It is true that more than half of these are the earlier
analysis of St. Claire Deville and Boussingault in which only
carbon and hydrogen were determined and the balance needed to
make 100 was assumed to be oxygen, but in a large number of
more recent analyses, both the sulphur and the nitrogen when
present have been directly determined and the balance then
ascribed to oxygen. Notably in Russian oils and Japanese oils,
both analysed in recent years and noting the sulphur and nitrogen,
has this presence of oxygen been recorded.

Rakusin (Die Untersuchung des Erdoels und seine Producte,
1906, p. yy) also quotes more recent analyses of Russian petroleums
by Charitschoff and by Xastjukoff. who tind from 0.4 to 2.5 per
cent of oxygen and, what is of interest, note that the percentage
of oxygen increases in the heavy petroleums and residues >vith
the specific gravity.

178

PRESENCE OF OXYGEN IN PETROLEUMS AND ASPHALTS 179

But we are not obliged to base our belief on the presence of
oxygen in petroleums on calculations made from ultimate analyses.
The discovery of the petroleum acids by Hell and Medinger in
Roumanian oils and phenols and of the naphthene-carboxylic acids
by Markownikoff and Oglobin has given us an explanation of the
presence of oxygen and justified the assumptions made from the
ultimate analyses.

With the natural asphalts, the case is different from that of
petroleums. Although earlier ultimate analyses of asphalts gave
large percentages of oxygen, it was because the presence of
sulphur in them had not been recognized and the oxygen was
supposed with the carbon and hydrogen to make up the ash-free
bitumen. However, Kohler (Chemie und Technologie der Natiir-
lichen und Kiinstlichen Asphalte, 1904, p. 81 ) gives several analyses
of natural asphalts by Day and Bryant and by Kayser in which a
small percentage of oxygen is given as present alongside of a
larger percentage of sulphur.

Both Clifford Richardson and Prof. S. F. Peckham, eminent
American authorities on asphalt, have taken the position that not
only is sulphur a distinctive element for natural asphalts, but
equally that oxygen is to be considered as foreign to natural
asphalts.

Besides the natural asphalts, we have also to note the artifi-
cial asphalts, obtained from petroleum, either by simple removal
of the volatile portions or by some form of treatment with oxygen
or sulphur at high temperatures. To the first class belong such
products as "D grade asphalt," made from California asphaltic
petroleum, (Clifford Richardson, The Modern Asphalt Pavement,
2d ed., 1908, p. 263) and "Baku Pitch" (Ibid, p. 271) and to the
second class Ventura Flux, Byerlite and Sarco Asphalt. Of these
last mentioned products Byerlite and Sarco Asphalt have been
made from liquid petroleum residuums by the action of a current
of air, either drawn through or forced through at temperatures
ranging from 380° F. (193.3° C.) to 500° F. (287.7° C.)

The action of the heated air may have two different effects
(see Hofer p. 85) according to temperature and rapidity or
quantity of air passed through. The oxygen may cause splitting
off of hydrogen in the form of water with condensation of the
hydrocarbons affected, or oxygen may be fixed, forming products

180 AMKR/CAX IXST/TiTE OF CHEMICAL EXGIXEERS

of oxidation which remain, in cither case rcsiihing in thick semi-
solid or solid products. Not only would it be very desirable from
a scientific point of view to determine which of these reactions
has taken place, or whether both have united in the formation
of the solid asphalt-like products obtained, but the matter has
been the subject of investigation in connection with patent litigation
over rival processes.

Of course, direct determinations of carbon, hydrogen, sulphur
and nitrogen may and do leave varying deticiencies to be charged
up to oxygen, but it would be desirable to be able to confirm
these calculations by a direct determination of the oxygen in the
product. No such method has thus far come into common use.
The method of Baumhauer, neither in its earlier form nor in its
later form, using a weighed quantity of dry silver iodate and
requiring first a current of hydrogen, then of nitrogen and finally
of hydrogen again, has not been favorably commented on by those
who have tried it. The method of Mitscherlich of burning with
mercuric oxide is also intended to give the oxygen at the same
time that the carbon arid hydrogen are obtained, but this method
does not seem to have worked satisfactorily in the hands of
those who have referred to it and has not been adopted by
chemists.

The process which I desire to present to those interested in this
subject is very simple in theory, although its execution is not free
from difficulties and requires time for its proper completion. It
is primarily, the invention of Dr. Wm. M. Cross, City Chemist of
Kansas City, Mo., with whose permission I have worked upon it
with a view of making it applicable to this class of products, and
to whose courtesy I am also indebted for the pemiission to give
publicity to these results. It consists in a combustion carried on
in a current of dried and purified hydrogen gas. the front
of the combustion tube being filled with iron wool, which, brought
up to a bright glow and thoroughly reduced by the hydrogen,
then acts as contact-substance and brings about complete reaction
between the hydrogen and the vapors given oflF from the decom-
posing petroleum or asphalt, whereby any oxygen present is taken
up in the form of water vapor passing on to be absorbed ultimately
in a weighed chloride of calcium tube. In making the determination,
hydrogen is passed very slowly through strong sulphuric acid, cal-

PRESEXCE OF OXYGEN IN PETROLEUMS AND ASPHALTS 181

cium chloride and over phosphorus pentoxide into the end of the
combustion tube containing the boat with the weighed asphah sample,
beyond which is a sufficiently long layer of iron wool. The com-
bustion tube at the farther end is connected with a good-sized U
tube containing purified asbestos wool or preferably spun glass
and this to a weighed chloride of calcium tube for absorbing water.
When the combustion furnace is first lighted, only that part of the
tube containing the iron wool is strongly heated, the part containing
the asphalt being kept cool. Hydrogen is then passed very slowly
through the apparatus until the chloride of calcium tube used for
collecting water has come to constant weight and so remained
for some time. The part of the tube containing the asphalt is
then increased in temperature very gradually until ultimately the
boat and its contents are heated to the maximum temperature
attainable and so held for a time. If the large U tube containing
the asbestos or glass-wool is kept cool, no condensable vapors pass
beyond, and if the current of hydrogen be continued a sufficient
length of time after the full heat has been applied, it will take
all water through as vapor into the weighed chloride of calcium
tube. No trouble need be anticipated from the small amount of
sulphur contained in the asphalt or petroleum product, because the
heated iron wool is capable of taking it up in whatever form it
is liberated.

After beginning my trial of the process with ordinary com-
bustion tubing, I was led by reason of the necessity of keeping
the portion of the tube containing the boat with the weighed
asphalt cool, while the portion containing the iron wool had to be
heated to a bright red heat, to try a tube of fused silica and have
found this to possess great advantages. With a tube of transparent
fused silica, some 30 inches in length, which I obtained from the
Silica Syndicate, Ltd., of London, Eng., the iron wool can be
brought to the desired heat, while the end of the tube containing
the boat can be kept perfectly cool by water trickling upon it. By
this means the rubber stoppers with which the ends of the com-
bustion tubes are fitted can also be kept cool so that no overheating
can take place.

I have not yet completed my analytical work upon the material
taken to try out the method and prefer to reserve a complete
illustration of the applicability of the method to both petroleums

182

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

and asphaltic substances for a fuller paper. I will, however, give
two oxygen determinations in a blown petroleum-residuum, or so-
called artificial asphalt.

Determination of Oxygen.

Weight of material taken

Water absorbed in CaClj tube ....
Corresponding weifihl of oxygen. . .
Percentage of o.xygen

1.0065
0.0440
0.0391
3 88

0.9767
0.0394
0.0350
3 58

DISCUSSION.

Prof. Edw. Hart: "I have had some experience in the determin-
ation of o.xygen in metallic iron by passing hydrogen over it at high
temperatures and I have very serious doubts of the success of the
method, which a careful reading of this paper shows has been
proposed by Dr. Sadtler, but not yet fully worked out. The use
of silica tubes with hydrogen is not an undertaking that one may
view without some apprehension in view of the fact that silica
does not hold hydrogen very well at high temperatures."

Dr. H. KipPENBERG : "The determination of oxygen in iron
cannot fairly be compared with the determination of oxygen in
organic substances, inasmuch as in the former case the accessi-
bility of hydrogen to the material is much more limited. Moreover,
if Dr. Hart says that silica tubes do not hold hydrogen very well
at high temperatures, this has no bearing in the case, since it is
not hydrogen but water that is to be determined. However, it
would be well if Dr. Sadtler could produce comparative figures,
for instance indirect analyses, proving the method of his direct
analysis to be fairly correct. It would also be well to give references
in regard to the findings of chemists of the practicability of the
Bauerhauer and Mitcherlich methods (page 4).

Dr. Sadtler: While I am not yet ready to publish complete
analyses of any of these oxygen-containing asplialts because the
matter is still withheld from publication on account of its being
connected with patent testimony, I can quote with regard to this
direct method the analysis of one other product in which I obtained

PRESENCE OF OXYGEN IN PETROLEUMS AND ASPHALTS 183

4.17 per cent of oxygen by difference. The chemist to whom I
referred in my article as having first proposed the process, Dr. Cross
obtained 4.14 per cent by difference, and the direct determination of
oxygen by this new process gave 4.01 per cent. I have since
obtained other results, but as before stated, the analyses cannot be
published as yet.

THE CHEMICAL ENGINEER AND INDUSTRIAL
EFFICIENCY

By \VM. M. BOOTH.

Read at the Detroit Meeting, December 6, 1912.

The chemical engineer can take liis legitimate place in industrial
affairs only when he begins to concern himself with values and
returns and can transpose the signs and symbols of the chemist
to the dollars, cents and percentages of the business world. The
profession must necessarily include men with diversified mental
attributes, experiences and education. Natural inventors, builders,
executives, analysts and economists are examples of the men who
will choose this branch of engineering as a life work.

The first and highest type of endeavor concerns itself with the
invention of new processes and their perfection, later establishing
useful industries. Relatively few men have the ability, courage
and means to embark in totally new enterprises, and the larger
percentage of those who do so, fail, because these three important
elements are not properly balanced.

Not less important, but demanding a different type of mind,
perhaps more strongly analytical in its nature, is the large and
ever increasing field open to those who are able to improve or
effect economies in the processes of firms already established.
Closely related to this is the examination of new enterprises that
seem to have merit and which need scientific assistance and capital
for development. No greater damage has ever been wrought on
American investors by any class of men than by the "new chemical,"
"private," or "secret process" promoters who have used the subtleties
of the science as a basis for fraud.

Irrespective of the particular division of endeavor undertaken,
the chemical engineer must fortify himself against all classes of
misrepresentation, and muse concern himself with questions of

184

THE' CHEMICAL ENGINEER AND INDUSTRIAL EFFICIENCY 185

process, cost, market, location and actual capital needed in any
new industrial enterprise. No considerable investment should ever
be made without a complete report from conservative men, who
are familiar with the industry involved.

While the basic operations of activity include agriculture,
mining, transportation and manufacturing, the latter is chosen as
best exhibiting the use of the chemical engineer along the lines
previously pointed out.

Those who have made a careful study of the splendid papers
of Dr. Monroe and Dr. McKenna to be found in the proceedings
of this Institute, have been impressed with the fact that nearly all
of the manufacturing of the United States is carried on east of the
Mississippi River, and that more than one-third of this is confined
to New York, New Jersey and Pennsylvania. The following census
report shows the increase in capital and people employed from 1850
to and including 1909:

Capital Invested in Manufacturing. Employees.

1850 $ 533,245,000 957.059

i860. . 1,009,856,000 1,311,246

1870. . 1,694,567,000 2,053,996

1880 2,790,273,000 2.732,59s

1890 6,525,051,000 4,251,535

1900 9,813,834,000 5,306,143

1910 18,428,270,000 6,615,046

It will be seen that the investment at the latter date amounts to
eighteen billion dollars and the number of employees to over six
millions. To maintain the almost perpendicular increase in our
manufacturing activities is the duty of the commonwealth, for no
more useful type of industrial activity can be found, especially
when our products can be placed in foreign markets at a profit.

The observations covered by this paper are necessarily personal
and have accumulated during 20 years, 10 of which have been
devoted mainly to the questions now to be discussed. The observa-
tions cover 53 "going" plants, representing 37 industries, and some
others that have never gone further than a prospectus distributed
by an ignorant or a dishonest promoter. Obviously, in a paper
of this kind, a general outline only can be given. The power plant
was discussed in my first and subsequent papers before the Institute.

In looking back over the vears covered, it would seem as though

186

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

the period has been one of unexpected crises, — rising wages,
unsettled market conditions, and acute competition. Among the
53 concerns above mentioned, there have been 8 failures, 2 have
withdrawn from business and i, only, has burned. The remaining
industries are owned as follows :

Private 1 1

Corporations 19

Trusts 12

The failures were attributed to the following causes:

Two to incorrect conceptions of the costs and profits of a

a business.
Two to dishonest employees.
Two to incompetent supervision.
One to insufficient working capital.
One to manipulation of the stock in New York City in

1907.

The superintendents of 20 plants have been forced out or dis-
charged for reasons such as inattention to duty, — incompetency, —
lack of knowledge of the business, — trust management, the intro-
duction of new methods, — inability to pay dividends on inflated
stock issue, — dissension among officers of the company, or inability
to handle help.

As I understand the matter, a general efficiency survey of any
business must recognize the following conditions :

External : Policy of the government toward an industry.

Capital upon which dividends must be earned.

Location.

Cost of plant and equipment..
Inlcrnal: Unit cost of finished product, subdivided as follows:

Raw materials

Supplies

Fixed charges : Interest

Labor

Office expenses

Depreciation

Power

Repairs

Insurance

Lighting

Sales

Taxes

Heating

Advertising

Cartage, freight and e.\prcss

Charity

THE CHEMICAL ENGINEER AND INDUSTRIAL EFFICIENCY 187

Considering the capital invested, and the importance of the
manufacturing business to all the people, — laborers, tradesmen and
stockholders, — the Government is bound to respect, foster and
protect these interests at all times. It would manifestly be suicidal
to introduce any highly protected industry into the United States
pending our tariff changes.

The passing of the pioneers who built and operated our first
mills has thrown the responsibility of management upon the
shoulders of many men totally unfitted by experience or temper-
ament to carry on the business. To add to this misfortune of
inheritance, all basic industries have expanded enormously, requir-
ing more capital than one family or group of men could furnish.
This led to the general adoption, between 1880 and 1900, of the
corporate idea. While of the greatest value as an industry builder,
no more pernicious influence has entered the manufacturing busi-
ness,— this conception and use of an artificial individual without
responsibility.

Abundance of money in the banks, the abuse of personal credit,
and easy bankruptcy laws have made it possible to squander the
people's money without scruple. In several instances in my e.xperi-
ience, good operating managers have attempted to maintain their
profits on an inflated and unwarranted stock issue, and have failed.
Good men, improved machinery and low operating costs cannot
off-set unnatural overhead expense. "Good will" has no place on
the balance sheet of a well-regulated and solvent business. Any
venture in the elaboration of raw materials ought, when brought to
a paying basis, to be able to return to the stockholders a net profit
of at least 10 per cent. Some old-established lines of business net
from 20 to 60 per cent annually, and two good years have often
paid for plant and equipment complete.

Considering now the matter of location; the manufacturers
generally follows his market. As the growth of the population of
the United States is westward, it has been found expedient to
move whole industries from Massachusetts and New York to
Michigan, Illinois and Missouri. Relocation of furniture and wagon
plants has been quite general, because it has been found cheaper
to ship the finished product to the markets than to bring the raw
material East. Changes in market conditions have compelled the
agricultural implement manufacturers to locate in the Middle

188 AMERICAN IXSTITUTF. OF CHEMICAL ENGINEERS

West. Formerly the manufacture of shoes was a Massachusetts
industry; now, whole towns in New York and Missouri are devoted
to this business.

No better illustration of economic change can be cited than
the conditions at my own birthplace, — a valley south of Utica,
N. Y. On a stream furnishing from 6o to 120 H.P. at each
plant, 16 mills were in operation from 1873 to 1885. These em-
ployed about 2000 people. Forks and hoes were made in 2 plants,
wagons in i. woolen cloth in 2, cotton cloth in 5, knit goods
in I, silk in i, paper in 2, and sewing machines and mowing
machines in i. The movement of freight and finished products kept
the railroad and scores of teams busy. Furnishing provisions for
the employees in the mills afforded a living for many tradesmen.

One agricultural implement plant was burned ; one was bought
by a trust and closed ; the paper mills have been idle for years ;
three cotton mills have gone out of business ; one woolen mill was
burned and the other was closed ; the knit goods plant and the
machinery plant burned ; and the silk industry was moved to Phila-
delphia. To-day, there are only three really good companies
operating in the valley. Originally humming with the whirr of
spindles and clicking with the throw of the shuttles in the looms,
the valley is now quiet, and agriculture is the main business. Those
of us who lived there did not know why so many fires took our
industries away. It was observed that no factories were rebuilt.
I now know that it no longer paid to make woolen and cotton cloth,
to spin silk, and manufacture paper in that locality. The peculiar
elements which we term economic conditions took our prosperity
away, with incalculable loss to all concerned. — stockholders, em-
ployees and tradesmen alike. The moss-grown walls to be seen
on many swiftly moving streams are monuments that mark
industrial change.

Capital is sometimes invested in new projects, the aim of
which is the use of raw materials that are suppo.sed to be abun-
dant, but that are later found to be insufficient in quality
or quantity. Cement plants along the Erie Canal in New York
State represent this class and also illustrate the rapid changes that
may enter the elaboration of a product. In this instance the use
of shale rock has taken the place of marl and clay in the manu-
facture of cement.

THE CHEMICAL ENGINEER AND INDUSTRIAL EFFICIENCY 189

Beet sugar factories were started at Lyons, Binghamton, and
at Rome, N. Y. The cost of the plant in each instance was very
large, people cheerfully investing their money, expecting unusual
returns to agriculture. After several years of failure and loss,
the entire project has been given up ; the empty buildings now
remain after an expenditure of not less than $2,000,000. Colorado
and California produce beet sugar at a profit. The location of
the industry in New York State was a mistake, but the stock-
holders had to learn this. In the meantime, canning factories have
sprung up throughout central and western New York and the
well-managed ones are in a flourishing condition. Cheap raw
materials, plenty of help, excellent transportation facilities and a
ready market are contributory causes to its success.

No science or art can determine with accuracy whether economic
conditions are correct for the location of an industry. Accident
or good business judgment may accomplish what statisticians and
scientists cannot.

Cost of Plant and Equipment. With plenty of money at his
disposal, the optimistic manufacturer is apt to spend too great a
portion on buildings and equipment. Ample working capital should-
always be held in reserve. The amount thus employed will
necessarily vary with the business, but from 23 to 50 per cent is
commonly set aside for this purpose in smaller 'industries, the
capitalization of which is from $50,000 to $200,000.

It is much better to build a plant in a modest way. anticipating
growth, than it is to find capital for running a concern in the
midst of business expansion; especially so, if stockholders have
had to wait from 3 to 5 years without dividends.

Again, a very expensive plant may be erected with consequent
large overhead expense, where the income does not warrant the
outlay. I found it impossible to recommend the erection of a water-
gas plant in a town of 3500 people. A canvass of all prospective
users showed that not more than 2 or 3 per cent income could be
expected. A similar plant in a town of about this number of people
can positively pay no more than 2 per cent on the investment after
all avenues for gas consumption have been thoroughly exploited.

Location. To aid those who wish to study the problems con-
cerning location, I have made a list of the elements that seem
important. These are as follows :

190 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

Atcessibility of raw materials Hygienic conditions

Market Taxes

Transportation Insurance

Labor Banking facilities

Power Heating

Water Lighting
Supplies
Climate

Obviously, all of these details cannot be discussed in a general
paper. The importance of one item, water, is taken up in the
second part of this communication, to show how carefully capital
should investigate a new location, when the growth of a business
warrants a change or when misfortune requires it.

With a favorable location, a demand for the product, an honest
.stock or bond issue, a modest initial outlay for buildings and equip-
ment, and sufificient capital for doing business, an executive should
earn a fair dividend on the investment.

Internal Unit Cost. The ideal is the basis of our best effort
■everywhere. In manufacturing, this ideal is approached when
the largest quantity of good goods is turned out at the lowest
possible cost. To determine how to attain the above conditions is
the duty of every executive. But the task is not a simple one, for
book keepers are not statisticians and although all of the data neces-
sary in connection with the proportioning of expense in the manu-
facture of an article may be derived, it takes a large amount of
study to draw correct conclusions. No simpler expedient in my
estimation has been devised in this connection than unit cost. What
does it cost to produce a pound, a horse-power, a barrel, a yard,
or a machine, — any single article, many of which are made each
month or year? -These items may be apportioned as percentages.
The separate items imder fixed and operating expense become fac-
tors of the total. As an example, we will say that the production
of a machine has entailed an outlay of $25.00 and that this is divided
as follows :

Raw materials 20%

Labor 40

Power 7

Lighting and heating I

Transportation 3

Office exfwnses 2.5

Repairs 1.3

THE CHEMICAL ENGINEER AND INDUSTRIAL EFFICIENCY 191

Sales lo

Advertising S

Charity 0.2

Interest, depredation, taxes, and insurance 10

This method shows at a glance that labor is a large item in
the cost of this article and that any economy that can be effected
in this department will make an appreciable saving in the total
outlay.

Through the kindness of Mr. E. Durand of the Bureau of
Census, I am able to present a comprehensive table illustrating the
method above outlined :

This is a valuable guide in any efficiency study of production
costs, although too many items are grouped under expense, which
may be used by any executive to conceal exorbitant bills of any
nature.

The actual cost of acase of tinned goods of the season of 1912
is divided as follows :

Raw materials 30

Labor 14

Fuel o

Freight and express o

Maintenance 4

Sales 3

Advertising , o

Interest i

Depreciation i

Taxes and insurance i

Boxes and labels 7

Loss on seed 5

Discount and brokerage 3

Expense 8

00%

The remaining items are not considered useful in this paper.
The tin container itself includes a cost of 85 per cent for materials
and 15 per cent for labor.

A woolen mill owner and operator furnishes the following
table :

Materials: Raw stock

Labor: Ofike

Expense

Insurance

Soap

Factory

Taxes

Dyes

Overseers

Charity

Wool

Executive salaries

Coal

Depreciation

Wool oil

Repairs

Cotton and shoddy

192

AM ERIC AX IXSTITUTE OF CHEMICAL EXGIXEERS

Statistics or Manufactcrf,. (Thirteenth Census, igio, page 30)

Per Cent of Total Expenses Itcported.

Salaries.

Wages.

Materials.

S-J

18.6

65.8

8.6

24-3

SII

4S

231

62. s

3-9

20.6

69.6

41

17-3

72.6

4.0

174

69.9

1-4

4-3

91 .0

5-6

^i 5

72.0

S-7

27.0

58.9

4 3

44.7

49.2

4-3

23.0

66.7

6.S

IS 0

68.2

5-2

20.7

579

6.0

23.0

61. 1

7-6

13 I

67.9

5-8

22.4

63 7

2.6

24.0

66.9

10. 0

24-5

53.8

i-S

2.6

92.8

8.7

29.8

50.1

7-3

308

51 0

10. g

18.4

46.2

4-4

=55

62.7

1.8

6.8

88.4

2.9

18.3

73-9

7.2

19-3

64.6

2.2

10 S

81.2

I.O

1.6

18.4

7.6

137

32.2

4.8

32.0

Sio

6.7

44.8

39-4

31

4-3

87.7

9 3

7-4

7t.i

4.0

17.2

69.7

14 9

8.7

44 1

1.8

4-4

89.6

16-7

26.6

32.6

4-2

21.8

60.8

i-S

3-9

91 3

0.7

3-8

94 4

0.9

3 4

94.8

0.9

2.8

92.6

4.6

19.0

48.4

2.6

18.7

72.9

6.4

2t.I

62.1

All industries

Agricultural implements

Automobiles, including bodies and parts

Boots, shoes, including cut slock and findings.

Brass and bronze products

Bread and other bakery products

Butter, cheese and condensed milk. . ,

Canning and preserving

Carriages, wagons, and materials

Cars, general shop construction and repairs by

steam railroad companies

Cars, steam railroad, not including operations of

railroad companies

Chemicals

Clothing, men's, including shirts

Clothing, women's

Confectionery

Copper, tin, and sheet-iron products

Cotton goods, including cotton small wares. . .

Electric mach., apparatus, and supplies

Flour mill and grist mill products

Foundry and machine shop products

Furniture and refrigerators

Gas, illuminating, and heating

Hosiery and knit goods

Iron and steel, blast furnaces

Iron and steel, steel works, and rolling mills. . .

Leather goods

Leather, tanned, curried, and finished

Liquors, distilled

Liquors, malt

Lumber and timber products

Marble and stone work

Oil, cottonseed and cake

Paint and varnish

Paper and wood pulp

Patent medicines, compounds, and druggists'

preparations

Petroleum, refining

Printing and publishing , .

Silk and silk goods

Slaughtering and meat packing

Smelting and refining, copper

Smelting and refining, lead

Sugar and molasses, not including beet-sugar . .

Tobacco manufactures

Woolen, worsted and felt goods and wool hats.
All other industries

THE CHEMICAL ENGINEER AND INDUSTRIAL EFFICIENCY 193

Percentages were not given but the total annual expense includ-
ing the three subdivisions above shown, is divided by the number
of yards of cloth turned out to determine the cost price per yard.

I am familiar with the actual cost of reducing a ton of garbage
by the naphtha process. This, on a percentage basis is as follows:

Labor 47-43%

Coal .' 20.81

Pressing 12-37

Filter cloth 2 . 89

Gasoline, oil, and light 8 . 00

Freight 1.77

Superintendent 3.97

Taxes 0.45

Interest 0.28

Office o . 24

Commissions and analyses o . 74

99-94%

Labor is shown to cost an excessive amount. The gasoline item
needs investigation.

The following elements compose the cost of a small copper
instrument :

Labor 61.62%

Raw materials 27 -41

Burner 6 . 03

Hanger 1.31

Polishing 1 . 64

Support 0.54

Paint 0.22

Screws 0.22

Lacquer o-SS

Bolts : 0.33

Solder o.ii

Obviously, the labor cost of the instrument is excessive.

The official having charge of the cost department should
ascertain at fixed intervals, by inventory and from records, the
exact unit cost of any or all articles produced. This information
should be made a part of a blue-print chart, carrying at the left
a list of the items composing the record and a continuous line,
showing the fluctuations in the cost of each, from month to month.
If any one of these lines rises from causes beyond the control of
the management, others must fall, if the price of the finished article

194 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

is to be maintained. Heating and lighting will fluctuate with
seasonal changes ; interest and depreciation, charity and office will
remain |)ractically horizontal. Unless the industry controls its own
raw materials these will usually increase in price; labor of all kinds
increases ; power is more expensive because coal is higher in price
and water power has in many plants been replaced by steam.
There is a very gradual rise in transportation costs and in supplies ;
taxes and insurance are constantly increasing everywhere.

With such records available, the operating manager is able to
determine where efficiency methods could be applied to advantage.

In a former paper before the Institute, I have discussed "Power"
from a percentage basis. Since that time, the use of electricity has
become ciuitc general and the H.P. year cost has been considerably
lowered in a large number of plants. The remainder of this paper
will be devoted to the purchasing and storing of supplies.

Stock and Supplies. The raw materials needed in operations of
the manufacturer are usually closely bought and economically
handled. I have found this particularly true in woolen, cotton and
paper mills.

Every successful enterprise requiring raw stock must include
an expert buyer of large experience, whose business it is to make
a study of market conditions and fluctuations. Ten years ago, much
more practical experience was required to fill such a position than
at present. This has been brought about by the general introduc-
tion and use of specifications. One by one, natural products have
been standardized ; coal, wool, cotton, ores, oils, paper stock, iron
and steel and natural earths; these are a few of the hundreds of
raw materials used by manufacturers. Physical and chemical stand-
ards have been set to replace the guess and estimation methods that
came from e.xperience and that are often wide of the truth. A
relatively inexpensive man, who has a testing laboratory at his dis-
posal can determine the actual value of raw stock much more
accurately than some high priced man can guess at it. Two items
on our cost sheet can be turned downward and kept there at
relatively small expense.

Unless the specification idea is carried throughout the mill to
include the finished product, the work is incomplete, for the adop-
tion of such a system invariably improves the c|uality of the goods
turned out. For example, every piece of wood, of composition and

THE CHEMICAL ENGINEER AND INDUSTRIAL EFFICIENCY 195

metal that goes into an automobile or locomotive should be of the
best quality, proved to be so by actual experiment. This rule holds
for manufactured products generally.

One of the weakest points in the personnel of the mill organiza-
tion to-day is the purchasing department. I refer more particularly
to those in charge of the purchase of the supplies. This important
branch of the business is often left to incompetent clerks, who
antagonize salesmen generally and who buy from men whom they
get the greatest possible return, — gifts, dinners, an occasional trip.
or even money. Honest traveling men avoid such purchasing
agents, to the permanent loss of the business.

A shrewd salesman may spend from six weeks to six months in
placing an order for expensive equipment that a concern never
needed and should not buy. In my experience, men totally remote
from the ordinary purchase of supplies should be employed in con-
nection with new and valuable equipment. Consulting engineers
can act to good advantage, turning in reports that show the general
market conditions, kinds of apparatus or material available, with
the experience obtained from the use of these in other plants.

Sjipplics. Every manufacturer uses mixtures and compounds
the exact nature of which he has no knowledge — oils, dyes, fillers,
adhesives, cleaning agents, waxes and polishes, powders and salts.
In some instances, such materials have a total cost of $2000 per
month. Many simple substances are sold in large quantities, at
inflated prices. For one concern, I was able to lower the cost of a
special substance brought for $50 a ton, by substituting the same
material from another source at $15 per ton. Good business
requires a knowledge of supplies and their component parts, for the
purposes of keeping the cost down, for the protection of workmen,
and to guard against fire.

No feature of factory economy should be as closely watched
as the storeroom. This should be separate, light, orderly
and so arranged that many articles varying in size and shape
can be found quickly. A store keeper should be in charge every
moment of the working day, and should be held responsible for
all stock handled, distributing this over a counter only, never allow-
ing workmen to come behind this. All orders should be signed by
proper authority and a carbon copy of each transaction kept. Tools,
in particular, and all stock that can be used about home, barn or

196 AMERICAN IXSTITUTE OF CHEMICAL ENGINEERS

garden will mysteriously leave the plant, a few cents worth at a
time, if a way is found to handle the inatter with an easy conscience.
Suiiunary. In the foregoing paper, 1 have attempted to point
out to you certain methods that can be adopted in the conduct of
any manufacturing business. The days of large profits, cheap raw
materials and labor have gone for good. With increasing prices
and competition, all executives must be economists as well. Effi-
ciency, in its broadest sense should include promotion, capitalization,
location, organization, ecjuipment and operation. Great stress has
been laid on the efficiency of labor to the exclusion of matters of
equal or greater moment. An exact knowledge of unit costs will re-
veal the weak points in any plant. The so-called efficiency engineer,
who spends three or four days in a concern and antagonizes every-
one from the bosses to the office boy, can accomplish little good.
Weeks and months of study are required to get at the details of
the business ; to make improvements is a still greater task. The
good-will of the employees must be gained and kept to make any
])rogress in economy studies. Discussion and argument naturally
follow any change in policy. The man who makes the change
should be on the ground to defend himself and drive home the facts
as he sees them.

WATER FOR INDUSTRIAL PURPOSES

By WM. M. BOOTH

Read at the Detroit Meeting, December 6, 1912.

Water Supply for the Manufacturer. Before locating a new
plant or industry, a large amount of preliminary information is
necessary. Having decided that market conditions, transportation,
labor and power are available and acceptable, a thorough study of
water conditions must be made. This should determine the quantity,
quality, and cost of this material necessary in the production of
power, for strictly manufacturing operations, for drinking, for
cleaning and for fire extinguishing purposes. Sum up all possible
requirements and add from 50 to 100 per cent for emergencies and
for growth.

If possible, two independent sources of supply should be obtain-
able.

Information of the character demanded can be obtained from a
commercial laboratory that has specialized in this direction, or from
a consulting engineer who has a laboratory at his disposal. Such a
study should be begun at least a year in advance of building oper-
ations. Seasonal changes are such that both quality and quantity
of water may vary greatly from month to month, if the proposed
source is a river, small stream or spring.

Having employed a man or company to make the necessary
observations and analyses, the proposed sites can be visited and the
requirements pointed out and discussed. If water is to furnish the
power of the mill and maximum and minimum flow data are not
available, they must be obtained from the government or from
original experiments conducted with a weir. Special forms of this
device are now sold with recording gauges that read in cubic feet
per second. If records have not been kept and the expense of the
instrument is more than is thought necessary, actual velocity and

197

198 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

depth studies can be undertaken at stated dates each month. If
the minimum of these readings shows tlie passage of the required
volume of water, the questions of quantity are dismissed for power,
fire and cleaning.

Such water is rarely exactly fitted for power and technical pur-
poses. There is, however, a considerable area of granite or related
rock in the United States, the run-off from which is soft and clean.
The Adirondacks, the White Mountains, and the Catskills all afford
an abundance of soft water. The plants along the streams running
from these mountains have many advantages due to this kind of
water supply. I have found the hardness to average about fifty
parts per million.

Shale rock areas in New York State at an altitude approximating
1400 feet also afford very good water, with a hardness between 100
and 120 parts per million. Limestone areas generally produce hard
water. Such a belt runs through the United States from eastern
New York to the Mississippi River and south, hardness 150-2000
parts per million. Before use in a power house, this class of water
should be softened by chemical means. The cost of treatment
varies from the fraction of i cent to 20 cents per thousand gal-
lons.

The quality requirements for manufacturing purposes vary with
the nature of the business. Textile mills demand a great volume
of soft water free from iron and sediment. Canned goods concerns
need a water under a hardness of 170 parts per million, clean and
sanitary, low in organic nitrogen. Power producers and steel plants
need large volumes of soft water, free from sediment and oil, and
cold for condensing purposes.

Many industries use water for rinsing. Laundries must avoid
water containing iron; in addition this should be soft and clean.
Nor can iron tanks be used in storing water for laundries; but
wood and concrete are always available.

In fact, very few operations of manufacturers require hard
water, and in such cases the necessities are generally well under-
stood.

If a stream cannot be appropriated for water supply, a lake
may be considered. The Great Lakes serve hundreds of plants.
The water has a hardness of from 90 to 120 parts per million. As
a cheap source of water of enormous volume they are unexcelled.

WATER FOR INDUSTRIAL PURPOSES 199

All lake water carries sediment which can be treated according to
the needs of the business. One grain of alum per gallon cleans the
usual run of lake water at a cost of less than $2.00 per million
gallons.

Smaller lakes in the Eastern States are usually on high ground
and necessitate a water works system between the source of supplj^
and the plant on the railroad. New York State includes within its
borders hundreds of such natural reservoirs. The water has a
hardness, approximately, of 100 parts per million.

Next to lakes, small streams and isolated springs may be con-
sidered. The annual maximum and minimum supply must be
definitely determined before any plans are made to use such water.
Large streams with a large average flow fifty years ago are often
dry in midsummer now.

Perhaps the industry does not need a large volume of water
daily, or must be situated in a town or city. When there is no
choice of location, bad water must be corrected mechanically or
chemically. If there is a choice between two or more towns, the
question from the water investigator's standpoint is what kind of a
supply and what equipment exists at each place.

A complete history of the water works company, plant and
equipment should be worked up, — short, but showing location and
extent of watershed, storage capacity, piping, pumping plant and
the financial standing of the company itself. The quality from a
sanitary, mineral and bacteriological standpoint should be made a
part of the record, — the result of personal investigation and not
from published records.

No modern mill superintendant can tolerate a scant supply or
a poor distribution system. We all know of towns where the water
pressure varies from 20 pounds to zero. Insurance rates are unduly
high and fire losses are numerous. Few small towns can supply
water in quantity sufficient for big business. My clients operating
canning factories require from 50,000 to 100,000 gallons of good
water per day for special uses ; woolen and cotton mills from
1,000,000 to 5,000,000 gallons per day; paper mills from 2,000,000
to 5,000,000. Canals and rivers flowing through towns are the only
inducements for large users. City water costs from 3 to 15 cents
per 1000 gallons ; 10 cents is not unusual. The bill for this item
alone may amount to $30 to $50 per day. Such a fixed factory

200

AMERICAN INSTITUTE OF CHEMICAL EXGIXEERS

cost is not unheard of but it cuts down profits with regular and
insistent demands.

If a town will furnish clean, soft water at lo cents per thousand
gallons to a concern using not more than 50.000 gallons a day, the
chances are that the use of such is desirable rather than an attempt
to find other sources with certain overhead expense and uncertain
results.

This statement apjilies also to wells, fully discussed in my pre-
vious paper before the Institute.

Drinking IVatcr. No two sanitarians will agree concerning the
standard to be set for potable water. In this paper I suggest three
types of water with possible limits of purity. Many thousands of
people are drinking each of the three grades daily, with apparently
no ill effects.

These tentative standards are as follows:

Parts per Million.

I. ' II. III.

0.02
0.08
1 .00
0.000
1.00
I .00
100.00
100.00
0.00
none
none
none
winter above

45° F.

summer below

60° r.

0 05

0.10

2.00

0.005
10 0

2 00
500.00
500.00
Presence in loc.c.
slight
slight

yes

40° F.
80° F.

0 IS
2.50

Nitrites

3-5
500-4000

Total solids . ...

B. coli

hea\-y
yes
yes

Odor

very cold
\cry hot

With increased attention to sanitary details everywhere, the
manufacturer can well afford to add a clean, pure supply to his
factory eciuipment. If it is impossible to obtain potable water, it
should be prepared. In case the supply is muddy, it should be
filtered; if polluted it should be passed through sand and charcoal
or distilled and then passed through charcoal. It must be remem-
bered that water distilled from an impre source, organically,
carries ammonia and sometimes other gases. Charcoal gives such

AMERICAX INSTITUTE OF CHEMICAL ENGINEERS 201

•water a pleasant taste and removes odor. Do not attempt to
condense steam from an ordinary boiler for drinking purposes.
Rather pass steam through a copper coil in a tin lined kettle. Con-
dense also in tin. Such water must be cooled before drinking.

When a manufacturing corporation can afford to do so, it should
build and operate its own water works. Ten, fifteen, or twenty
miles is not a prohibitive distance to go for a good supply. The
initial expense will be small compared with the additional resources
of the plant that has all of the clean, soft water needed.

To accomplish such a purpose, it may be necessary to buy
several hundred acres of cheap land. This should be fenced and
all people and animals kept out. Having an abundant supply, a
corporation may add to its income by selling water.

If water of a poor quality, but soft, is available near the
concern, a purification plant on a large scale can be built to good
advantage. Here water may be filtered or softened to the degree
required by the average use to which it is put.

DISCUSSION.

President : Gentlemen, Mr. Booth has presented to us a lot of
simple facts which although self-evident to many of us, are unfortu-
nately very often overlooked, especially by chemists. I personally
remember very well an incident where electrical power was offered
by two localities. In one it was oft'ered at a price of 50 per cent
below that of the other, and the amount of power under consider-
ation was about ten thousand horsepower, which meant a difference
of many thousand dollars a year for the cost of power, and yet it
took fully two months of calculation and investigation in order to
find that the power which would initially cost so many thousand
dollars a year more, was finally the cheaper, because unavoidable
interruptions of the cheaper power swallowed up the general effici-
ency, so as to offset any initial benefit of cheaper power rates. There
is one subject, which Mr. Booth has not mentioned, and which in
some instances has caused considerable trouble, namely, the trans-
plantation in this coimtry of foreign industries raised and developed
in Europe. For instance, industries which have been successfully
carried on in England, France and Germany and which were tried
in this country with practically no doubt as to their success, because

202 AUERJCAS J.\STirLT£ OF CBEUICAL ESCISEERS

the promoters believed the conditions here would be the same, and
where the enterprises did not succeed because the originators did
not take into consideration the extreme changes in the climatic
conditions of our seasons. In winter time we have an unusually
dry climate, incomparably drier than in lingland or the European
continent. Then again, in summer time, some industries are impos-
sible here on account of abnormally high dewpoint or exaggerated
amounts of humidity in the air. Around New York in July and
August, and even during the first days of September, there are times
when the dewpwint goes as high as 70° to 74° F. Such extreme
conditions of temperature and dewpoint are practically unknown
in Europe.

We still have a few minutes to discuss this subject. Is there any-
bo<ly who desires to make some remarks.

Prof. Bartow : I would like to say a word in regard to the second
part of the paper. I think the suggestions in regard to the need of
good water supply is important. I have recently had my attention
called to a factor}^ located in a town where the city authorities
agreed to furnish them all the water they wanted, and did not take
into consideration the fact that this one factory would need more
water than the whole city supply, and the fact that the city was
it.self quite short of water. Also the lack at times of appreciation
on the part of municipal authorities and others is sometimes brought
out when, for example, the mayor of a city states that he does not
believe that a good water supply can be furnished through city
mains, and when he goes to cities with different water from his own
town (he. by the way, does not have good water in his own town"*,
he cannot drink, and sajs that he would never in any town drink
the water which was furnished, no matter how good it might be.

Mr. Booth : There is a business which is on very good footing
in Sweden, and a man of my acquaintance went abroad and brought
back samples, and interested 30 men, and I was one of the unfortu-
nate 30 men who invested some of my money to help start that
industry in this country, capitalizing for a hundred thousand dol-
lars, $63,000 paid in, and we put up a building and had $18,000, to
put in the business. We had no market in this countr}-. and
endeavored to start a market. The $18,000 disappeared, and then
they came to me and said. "Your stock is no good, and we will pay
30 cents on the dollar for it." The concern failed, and I was glad

WATER FOR INDUSTRIAL PURPOSES 203

to get that out of it. It only goes to show what the dangers in
manufacturing are. The point in my paper is that manufacturing
is an enormous and growing business. It has a future in this
country. The efficiency of the mines is going down, as far as the
amount of gold that we can get out of the earth is concerned. That
line is going down, and one of the greatest industries, manufactur-
ing and inventions, must replace what we have lost in the natural
resources, and so I am bringing to you chemists and chemical
engineers something which you should be interested in, as chemists,
and as inventors.

There is one point which deserves careful consideration by all
having experience in business matters ; that is, that the best business
can be swallowed up by over-capitalization, and that very often
happens in this country. There is no limit to the amount of water
you can pump into any organization, and many people, especially
chemists, do not always realize that, however good a proposition may
be, it can be simply annihilated by the unscrupulous promoter who
pumps in water and wants to capitalize everything in it, and then
leaves the whole thing high and dry, and then you must wait until
bankruptcy sets in, and all the time you have become lukewarm, on
a very good enterprise, which for this reason becomes impossible.
For instance, inventors having a patent or invention to sell, often
do not realize that there is a limit to the value of an idea or inven-
tion. The best patent in the world is not worth more than a certain
amount of money, and the most extravagant starts have been made
in some industries, and that is mainly due to the fact that the super-
vision of the firms or incorporations in this country is very imperfect
as compared with Germany. In Germany you cannot begin to
capitalize everything — water, air, pipe dreams and rain drops. In
some cases where firms pay a very fair sum of money for a patent,
the patent is put down right away in the assets, "Value i mark,"
because if they did not do so the state would have said, "Well, you
put that patent valuation 12,000,000 marks, now where is that
value?" That would have deducted from the profits. It was better
to start with a valuation of i mark. When people begin to speak
of good will and the supposed value of a patent, there is no limit to
the imagination of a promoter, which is generally very abundantly
supplied, especially if the patent is the main commodity, with which
to get the money of some people into his hands.

THE AVAILABILITY OF BLAST FURNACE SLAG
AS A MATERIAL FOR BUILDING BRICK »

By ALIiERT E. WHITE.

Of the University of,Michigan.

Read at the Detroit Meeting, December 4, 1912.

There are three main prockicts made in a blast furnace ; one is
pig iron, another is the so-called waste gas, and the third is slag.
The first of these products meets a ready market and is the
primary object of the smelting operation. The second of these
products, the waste gases, have of late years been the recipients
of a considerable amount of study looking to their complete utiliza-
. tion. Waste gases have been used for many years in. heating hot
blast stoves, which in turn preheat the air blast which enters the
furnace. Only about one-third of the energ)' of the gas is used
in this manner. The remaining two-thirds of the energy in the
gas is already partly utilized and will probably be ultimately almost
completely converted into power, through the agency of gas engines.

But how shall the slag be utilized? \"arious methods have
been proposed for its efficient utilization, but none, at the present
time, have received any great amount of approval. This, at least,
applies to those methods which have aimed to utilize the great bulk
of the slag.

The production of blast furnace slag in the United States at
the present time is about 32,000,000 tons a year. The significance
of this figure becomes more apparent when we consider that it is
almost as great as the tonnage of steel produced.

The most important single utilization of the slag is as one of
the raw materials entering into the composition of Portland cement.
This industry cannot well utilize, however, the slag obtained at
the time of casting because such slag carries small iron particles.
Nor can it use to advantage slag high in sulphur, or of unsuitable
1 Permission must be obtained from the author for making abstract or
reproduction of this article.

204

BLAST FURNACE SLAG AS MATERIAL FOR BUILDING BRICK 205

composition. These conditions probably render it difficult to use
over one-third of the slag in cement manufacture.

The annual production of cement in this country is about
75,000,000 barrels of 380 pounds each which amounts to 14,250,000
tons. Portland cement made with slag carries roughly 50 per cent
of its weight in slag material so that one-half of the weight of
cement made in this manner represents the weight of the slag which
could be thus used, which is 7,125,000 tons.

According to the estimate given above one-third of all the
slag or 10,000,000 tons might be used for this purpose. This means
that the cement output of the United States might increase 50 per
cent and all of it be made in part from slag while still using only
one-third of our present slag production. Although the produc-
tion of cement composed in part of slag is steadily increasing, it is
not at all probable that it. will ever displace clay and shale altogether
as raw materials.

It was also suggested, at one time, that slag spaulls would make
good railroad ballast, but, after 10 or 15 years of trial, the rail-
roads have rejected this material because of the tendency of certain
slags to fall to powder and cause a dust nuisance to the travelling
public and, worse than this, numerous and serious track troubles.

Slag can readily be converted into mineral wool, but from the
tonnage standpoint there is an annual demand for but a relatively
small quantity of this material and thus one can easily appreciate
from this same point of view how really insignificant is such a
utilization.

When the problem was first given to the writer for investigation
by a firm with whom this question is a live one, he was cautioned
that the utilization he should propose must be one which would
use a large tonnage. The one at first glance which presented the
best possibilities was that of converting slag into a paving brick.
Good paving brick is made from the slag of certain blast furnaces
in England and on the Continent by casting the slag into blocks
and annealing the product. Many attempts were made by the
writer to convert the slag at his disposal into paving bricks but all
attempts were failures. Some of the bricks broke up on cooling
and those which remained sound were so brittle that they would
usually break if dropped on the floor. The reason for this failure
to make goo^ paving bricks is not yet thoroughly understood. Mr.

206 AilERICAX INSTITUTE OF CUEMICAL ENGINEERS

E. C. E. Lord, I'etrographer for the United States Government,
has been working on the mineral constituents of slag for a number
of years attempting to determine why the slag made in the blast
furnaces of the United States cannot be made into a paving
brick. So far as the writer is aware Mr. Lord has not yet been
able to suggest a method of furnace operation feasible under
American commercial conditions which will produce slag suitable
for slag paving bricks.

It seemed more promising to attempt to use slag in com-
bination with a small percentage of lime as a building brick, in a
jirocess similar to that employed in the manufacture of sand-lime
brick. As at least 95 per cent of the constituents of the brick
would be slag there was but little question but that, if successful,
the process would afford an outlet for a large tonnage of slag.

The process in general for the production of slag-lime bricks
should be nearly identical to that employed in the production of
sand-lime bricks. Since this latter process is more or less well
understood time will not be taken to go into details regarding it.
One can readily comprehend that there is nothing essentially new
about the idea. Because of the small quantity of slag-lime bricks
made it was not possible to follow out in its entirety the standard
sand-lime brick process. Since this was so, the method used in
making these slag-lime bricks will be outlined.

The slag as it came molten from the furnace was dropped from
the slag trough through jets of water into a granulating pit in
accordance with usual practice. The finely granulated slag
shovelled from this pit was dried and shipped to one of the most
modem sand-lime brick plants in the country where the experimental
slag-lime bricks were made. It was recognized that there would
be no difficulty in getting combination between the lime and the
slag, for slag is more reactive than sand. The question resolved
itself into so correlating the grain size of the slag particles and
the pressure employed in forming the brick as to get a finished
brick of best physical properties. Eleven sets of brick were made.
There were six sets in Lot i, and in the main all six sets were of
nearly identical composition and structure. There were two sets in
Lot 2. These differed chiefly from Lot i bricks in the amount
of pressure to which they were subjected for Lot i bricks were
made under a considerably greater pressure than Lot 2 bricks. In

BLAST FURNACE SLAG AS MATERIAL FOR BUILDING BRICK 207

Lot 3 are found three sets of brick. This was the last lot of bricks
made and the experience gained in the making of the first two
lots proved of great value. For this reason the quality of the
slag-lime bricks in this lot was superior to that of the bricks found
in Lots I and 2. Because of these conditions the data relating
to the composition and method of manufacture of Lot 3 bricks
has been chosen rather than the data of either of the other two
lots.

The lime and finely granulated slag were reduced to fine powder
by grinding in a ball mill. A portion of the coarse granulated
slag and, in addition, in one of the tests, some river sand, was
then mixed with these ground products. A rough sizing of the
constituents of the three sets of bricks found in Lot 3 gave the
following results :

K.

Lime, finely ground .
Slag, finely ground. .

" on 30 mesh . . .

" on 40 mesh . . .
River sand ........

7 3^
34-4
58.3

34-4
S8-4

10.0%

35°

50.0

A small amount of water was then added to the mixture. The
material was then fed into the brick machine and in this series in
such volumes as to give the maximum pressure which the brick
would stand without its showing air cracks when removed from
the press. They were steamed for 10 hours at a pressure of 125
pounds per square inch.

Their analysis is as follows :

Analysis of Lot 3 Bricks

Fe....
FesOs. .
Mn.. ..
SiOs . . .
AI2O3. .
CaO...
MgO..

S

Miss'n^

I.

J.

K.

i.6s%

1-55%

I 50%

0

70

0

92

0.63

I

08

I

08

1 .02

30

69

3i

28

34 87

15

04

14

16

1537

44

t>5

43

81

41.17

4

01

3

45

4.06

I

13

I

29

1. 16

I

05

0

46

0. 22

208 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

The bricks thus made were of a pleasing bluish-gray color.
The average weight was somewhat less than a sand-lime brick or
a common clay brick of the same volume.

Tin; Test Proper.

Method of carrying out tests. The results obtained and some
conclusions to he drawn from these results. — A (luestion of prime
importance in regard to this proposed slag utilization is one that
pertains to the quality of the slag-lime brick. As one familiar
with the brick industry realizes, there are no standard specifica-
tions for testing bricks and likewise there are even a few, who
ridicule the advisability of any specifications. For this investiga-
tion the brick testing specifications of Mr. A. \'. I'leininger, Chief
of the Ceramic Division of the U. S. Bureau of Mines, were em-
ployed. These specifications include compression tests on bricks
free from moisture but otherwise untreated, compression tests on
bricks saturated with water, compression tests on bricks which
had been frozen while wet and subsequently dried, compression
tests on bricks which had been subjected to fire and afterwards
air-cooled, and likewise compression tests on bricks which had
been subjected to fire and immediately quenched in water. They
include a transverse test on bricks which had previously been
subjected to the conditions set forth in the compression test and
an absorption test on the bricks. A determination of the weight
of each type of brick in pounds per cubic foot was also made.

The data on the I. J. K. series of slag-lime bricks or the bricks
of Lot 3 are reproduced herewith and for comparison the variation
from the standard set by Bleininger for standard building brick.
Neither the fire nor freezing tests were made on this series.

Regarding the test as a whole it can be stated that comparison
may now be made between the 14 sets of slag-lime brick which,
as previously stated and explained are grouped into three lots,
and various other forms of building bricks. All the tests here
quoted were carried out under the author's direction in order that
the results might be comparable. The various forms of commercial
building bricks consisted of three different lots of sand-lime bricks,
one of common clay brick, two of vitrified building brick, and one of
repressed brick. The figures are given as an appendix in Tables I,

BLAST FURNACE SLAG AS MATERIAL FOR BUILDING BRICK 209

Series of Slag-lime Bricks.

Average weight of brick in pounds per cubii foot
Transverse test on untreated brick. Modulus

of rupture

Transverse test on brick saturated with water

Modulus of rupture

Compression test on untreated brick. Strength

in pounds per square inch

Compression test on brick saturated with water.

Strength in pounds per square inch

Per cent of water absorbed

425

2500

2000
20.0

"3

500
4385

2970
iS-3

109
441
429
4026

2733
17-5

97

383

443

4580

3179
19.7

II, III, and IV. The results are shown graphically in Plates i, 2,
and 3.

The vitrified and repressed bricks are not of the same class
as are the common clay, sand-lime, and slag-lime bricks but the
results are included because of their interest. The direct and
essential comparisons should be between a theoretical brick just
within the bounds of specifications, a sand-lime brick, a common
clay brick, and a slag-lime brick.

It is noted that in practically all cases the common clay brick
is superior to both the sand-lime and slag-lime bricks. This is due
to the fact that the clay from which these bricks were made is of
as high a grade as any common building clay found in the United
States. It is also noted that in practically all cases the sand-lime
brick is superior to the slag-lime brick. In some measure this is
due to the fact that the sand-lime bricks had been allowed to set
for 6 months after their steam bath while the slag-lime bricks
were but 6 weeks old. Another reason manifest for the poorer
quality of the slag-lime bricks is because of the void question.
Granulated slag— these bricks were made from granulated slag —
contains about 52 per cent voids. Fine crushing, even to a point
which permits all of the product to pass through an 80 mesh screen
does not eliminate all of this trouble. A microscopical examination
of the ground slag dust discloses the fact that much of the dust
is a hollow spherical mass. This hollowness of the particle makes
it structurally weak. Since this investigation was first performed
the writer has been considering various means for meeting this

210 AMERICAX IXSnrUTE OF CHEMICAL EXGl\EERS

difficulty as efficiently and effectively as possible. He feels that
were slowly cooled slag or slag cooled en masse used, instead of
granulated, or water, or air cotiled slag, there would be manifested
a noticeable improvement in the quality of the brick. The results
of the tests on the slag-lime bricks seem to bear the writer out
in this theory. The materials in the bricks of Lot 3 were ground
finer than the materials in the bricks of Lot i and Lot 2. In all cases
Lot 3 bricks were superior. The constituents in the bricks in Lot
I were pressed harder than the constituents in the bricks of Lot
2. In all essential places Lot i bricks are superior to Lot 2
bricks. Greater pressure and finer grinding have helped to remove
the globular nature of the slag. Thus the better (juality of one
lot of slag-lime bricks over that of another is accounted for.

It is observable that the freezing test made practically no im-
pression on any of the bricks. It is not believed that such a result
was due to the fact that all the bricks tested were impregnable to
5uch a te.st. It is felt that the test was not effective for it was
not possible at the time the test was made to go below 20° F.
whereas the standard temperature for the test is 15° F. After the
freezing, each brick was put into a drying oven for the purpose
of driving out all free moisture. Thus one would expect to get
concordant results with those that were obtained on bricks free
of moisture, but. in other respects, uiureated. This was what
proved to be the case.

It has been asserted that lime bond bricks have much better
fire resisting properties than other tN'pes of building bricks. This
may be true when the bricks are en masse. It was not true in
this case when the bricks were subjected individually to a fire
test. In all cases the lime bond bricks swelled batlly. cracked, and
spauUed, so that, in many cases, it was impossible to test them.
This was particularly true of the slag-lime bricks.

It would be interesting to give the complete results of the
absorption test. At the present writing, however, the only figures
at hand are those which show the absorptive power of the various
bricks at the end of 48 hours. .Mthough the slag-lime bricks absorb
a greater percentage of water than the other bricks, they can be
made, and. in the cases of Lot i and Lot 3. were made to be within
the specifications. Common clay bricks usually absorb their full
amount of water within an hour. Tlie lime bond bricks absorb

BLAST FCRffACE SLAG AS MATERIAL FOR BUtLDISG BRICK 211

water much more slowly and gradually. This characteriitx. many
believe, is not for the best. Yet, it is true, that alter 36 hours
have elapsed no further absorption is noticeable in the bricks. In
all cases when properly made, the maximum absorption of slag-
lime bricks is under 20 per cent, the figure which is mentioned in
the specifications.

The result of these tests indicated that the slag-lime bricks were
inferior in every respect to the sand-lime bricks, and likewise that
they were vastly inferior in every way to the red clay building brick
found in the district where these tests were made. By inferior it is
not meant to imply that the slag-lime brick was below standard
specifications. For the most part it was not, and in those particular
instances where it did not come up to the stanrJard, the conditions
which brought these defects about can be so remedied as to raise
the standard of the brick up to and above the required amount.
With regard to the slag-lime bricks, however, it is not a
question as to whether they can be made to pass requirements,
so much as it is a question of a comparison of their quality with
the quality of the bricks which are made in the same district. In
the district where this particular test was made the building bricks
are of an unusually high grade. They are of a high grade because
the manufacturers have no difficulty in making a high grade brick,
due, quite largely, if not altogether, to the fact that the clay with
which the brick makers are working is, for the purpose, of as
fine a quality as is found in the United States.

When one goes to other districts, however, conditions are
found to be different. The bricks in the Philadelphia district. New
York district, Chicago, and Detroit districts and in almost all parts
of the South and West are known to be uniformly poor. This
condition is due quite largely ; to the fact that the brick manufac-
turers do not have a very good quality of clay to start with. In
such districts the slag-lime brick would have an excellent chance
of surpassing in quality the grades of common clay building brick
which are at present found on these markets. If there are blast
furnaces in these districts finding difficulty in economically dis-
posing of their slag, it impresses the writer that the conversion
of their present waste product into a slag-lime brick would be a
question worthy of careful consideration, in as much as slag-lime
bricks can be made as cheaply as other kinds of bricks and like-

212 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

wise in as much as the quality of the resultant brick would be
superior to that now on the market.

It is of course understood that it would not prove to be practi-
cable to ship slag-lime bricks any great distance any more than it
is practicable at the present time to ship the ordinary building
brick a considerable distance. The question of freight rates enters
into the commercial consideration of this problem and thus, to
a certain extent, limits the range of this utilization.

Thus, one can see that the (]uestion of converting slag into
slag-lime bricks is not one possessing uncertainties as to whether
or not a slag-lime brick can be made. That question has been
settled and slag-lime bricks can be made and produced as cheaply,
it is believed, as any type of building brick at present on the
market. It is not known whether or not the slag-lime brick will
deteriorate under long service. This point can only be settled by
a long time test. From the manufacturing standpoint it is a
question of local consideration around the immediate vicinity of
each blast furnace or group of blast furnaces. If the demand for
bricks is large, if the grade of bricks at present made are poor
because of an initial poor quality of clay, and if there is no ready
outlet for the disposition of the slag, it would then behoove a
blast furnace manager to consider seriously such a utilization.

BLAST J'URN ACE SLAG AS MATERIAL FOR BUILDING BRICK 213

TABLE I

Summary of Tests on Various T^tes or Building Bricks

Kind of Brick.

Weight of
Brick per
Cubic Foot
II Pounds.

Variance
with Re-
quirements
ic Per Cent

Sand lime .

Average

Slag lime. Lot i .

Average

Slag lime, Lot 2.

Average

Slag lime, Lot 3 .

Average .

Common clay. . . .
No. I. Repressed.
No. 2. Vitrified. .
No. I. " ..

107.6
no. 7
6
3

825
6S7

357
418
413
421
44S

358
351
355

565
441
383
463

1935
16-39

362
3°4
461
376

273
236
252
212
243

239

221
230

.500
429
443
457

I142
876
1456
1413

214

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

TABLE II
Summary of Tests os Various Types op Building Bricks

Tranaveree Teat.

Saturated with

Originally Brick F

ubjected to Fire.

Water Frojcn.
Then Dried.

Kind of Brick.

Type

Air Cooled.

Water Quenched.

Variance

Variance

Variance

Modulua

with

Modulus

with

Modulus with

of

Require-

of

Require-

of Rcquire-

Rupture.

ments in Rupture.

ments in

Rupture. ment.t in

Per Cent.

Per Cent.

Per Cent.

Sand lime

I

618

125.0

No fire t

ests were

made oni this lot

"

2

607

121. 8

"

"

"

"

"

i

■762

177 0

"

"

"

"

Average

662

141 . 2

"

"

"

**

Slag lime, Lot i . . .

A
B
C
D
E
F

419
SH
434
268
314

52 4

86.9

S7.8

2 5

14.2

"

''

,.

•'

Average

390

41 .6

"

"

*'

'*

Slag lime, Lot 2 . . .

G
H

22s
266

18.2
3 3

.,

"

"

"

Average

246

10.7

**

**

' '

"

Slag lime, Lot 3 . . .

I
J
K

No f reez

ing or fir

e tests w

ere made

on this lo

t of brick

Common clay

1244

352 0

182

263

184

266

No. I. Repressed. .

1254

3S6 8

310

520

310

S20

No. 2. Vitrified. ..

1806

3568

8S

70

89

78

No. I . " ....

1829

565 0

310

520

3>o

520

BLASZ FURNACE SLAG AS MATERIAL FOR BUILDING BRICK 215

TABLE III
Summary of Tests on Various Types of Building Bricks

Compression Test. (Expressed in Pounds per Squ

Saturated withWater

Frozen. Then

Dried.

Require-
ments in
Per Cent.

Crushing
Strength.

Crushing
Strength.

Require-
ments in
Per Cent.

Sand lime .

Average

Slag lime, Lot

Average

Slag lime, Lot 2

Average

Slag lime, Lot 3

Average .

Common clay.
No. I. Repressed
No. 2. Vitrified.
No. I. " .

Q083
7158
9402

3027
3803
3754
2454
2858
3463
3227

2203
2104
2154

438s
4026
4580
4380

7043
8567
11165
11138

262
187
276

242

75
61
83
73

182
247
347
345

5563
4q88
7025
5859

2171
3516
2662
i960
1632

2388

1475
1366
1421

2970
2733
3179
2961

8197
7680
8197

178
ISO
251
193

310
32s

8738

3149
4737
3324
2556

3346

2362
2512
2437

No freez
madeo

6522
8573
10608
1 1366

38s
286
470
380

75
163
85
42
59

8S

ing test
n this lot

264
376

216

AMERICAN INSTITUTE. OF CUEMICAL ENGINEERS

TABLE IV
Summary of Tests on Various Types or Building Bricks

Kind of Brick.

Type
Brick.

Compression Test. (Expressed io

Pounds per Square Inch.)
Originally Brick Subjected to Fire.

Air Cooled.

Variance

I Crushing r.'!;''>„.

Strength. I R^^2uT„

I Per Cent.

Water Quenched.

Crushing
Strength.

Variance

with
Require-
ments in
Per Cent,

Absorption Test.

Total
Absorp-
tion in
Per Cent,

Require-
ments in
Per Cent.

Sand lime.

Average

Slag lime, Lot i

Average

Slag lime. Lot 2

Average

Slag lime. Lot 3

Average .

Common clay
No. I. Repressed
No. 2. Vitrified.

No. I.

3362
2484
3395
3080

1535
2972
2102
Broke

1472
1326
1399

5850
8653
9095
i°309

26. s

380
411

477

4488
Broke

1496

3126
4045
3992
Broke

Broke

6297
7905
8882
1 1 270

72
124
122

243
335
401

526

»4-5
131
13 9
13.8

18.9
16.7
16.0
16.7
18.6

17-4

25.2
24.0
24.6

15 3
17-5
19.7

27
34
30
30

SS
16
20
16

7

BLAST FURNACE SLAG AS MATERIAL FOR BUILDING BRICK 217

--

:t =

C2=

^^

-^

B

rick

Sym

bols

1

^9rH

•3

Slas-iLime

Lot 1

3

Slag-Lime

Lot 2

fit

Slae-Lime

Lots

Sand-Lime

■s

s

Common Clay

'^ 18

L.-.T^

_^

No. 1 Vitrified

c

%

_..._

^-^

No.i

Vitr

fied

!S

No.

Rep

essed

<!

H

!>S

Plate I. — Weight and Absorption Tests on Building Bricks.

218

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

1

Brick

Symbols

Standard

Slag

Lime

Lot 1

.._.,

Slas

Lime

Lot 2

Slag

Lime

Lots

Sand

Lime

_i ^

No.1

Vitrified

^ ^

Na2

Vitrii

ed

Common C

ay

No.1

Repr

ssed

y

.^

uooo

10000

J5

X

<

/

■*"-

^

'^

"^

^^

y

^

X

^

V . ,

^

^j

A

*" "

\

7000 A

>^

■^

'^-

<

\
\

k

y

y

\

-^

\

S

^

^

\

"^

-^

..^

■\

\

m

- —

~— -

-.-

' '

-■

^.

\

"

r^'

---

■■-"

■

-~.>.

<;'

'^'~~

1000
0

■•>

" -^

Free
Mois

ture

St

turat
Wa

id wit

ter

Ji

Sa

urat<
Wa

dwit
ter

I

Or

^nal

Bricl
to 1

Subjected
"ire 1

Fro
Then

zen
Driec

A

ir Cot

led -

WaU

rQ„«

Dcbed

Plate II. — Compression Tests on Building Bricks.

BLAST FURNACE SLAG AS MATERIAL FOR BUILDING BRICK 219

1

Brick £

1

ymbpis

Stan

iard

Slae

Lime

Lot 1

Slas Lime

Lot 2

1
Slag Lime

Lot 3

Sand

Lime

Common C

lay

J_

No.1

Vitri

ied

\>- -«-

No.2

Vitrified

No.l

Repr

issed

2000

V

^

^

^^

\

^^

X

•^

^'

^

\

V

V,

^\

1

"

.^

s,

•8

....

••••

.•■'

\--

^v

3

-^

\

\'

SOOg

600

:>.,

— --

^-'

""

\

^^

400

- —

■-^

j".-^ —

^

— —

•"

-^

V

—

—

-■ —

,

1

V

_,_

II

,

0

Free
Mois

'rom
ure

Si

turat
Wa

:d wi'
ter

h

Sat

urated witl
Water

Or

ginal

Brick
to F

Subj

jcted

Frozen
Then Dried

i

ir Co

oled

Wat.

rQu.

nched

Plate III. — Transverse Tests on Building Bricks.

TECHNICAL ACCOUNTING AND CHEMICAL
CONTROL IN SUGAR MANUFACTURE

11} DAVID I-. DATOIX, Jr.

Read at the Detroit Meeting, Dee. 6, 1912.
Introduction.

For the technical supervision of the nianiifacture of sugar,
whether from beet or cane or whether the purpose be to make
raw sugar or retined granulated, the activities of the chemist may
well be directed along three lines of endeavor.

First, the sampling and analysis of all raw material such as
coal, coke and limestone or lime. Almost without e.xception in
the beet industry and in exceptional cases with the cane, this
includes the daily systematic valuation of beets and sugar-cane
deliveries for purposes of purchase. Further it will include the
analysis of field samples to determine maturity of crop in general
and the effect of certain influencing factors in particular districts.

Second, the frec|uent and rapid testing of initial material, inter-
mediate products at the several "stations" of manufacture and the
final products, together constituting what is known as "chemical
control."

Third, the keeping of the sugar account and the daily calcula-
tion of the efficiency of the various pieces of machinery and of the
several intermediate processes of manufacture.

Chemical control is essentially diagnostic in character and takes
advantage of the knowledge we have of how the sugar-bearing
material should behave at the "stations" as now interpreted through
chemical tests and of what constitutes recognized, unavoidable
losses, to put in the hands of the foremen in charge the proper
data.

Successful sugar accounting calls for good organization first

220

'CHEMICAL CONTROL IN SUGAR MANUFACTURE 221

and conscientious, well-trained chemists to carry it out. Success
or failure depends upon the presence or absence of suitable con-
veniences, accurate factory weights and measures, calibration of
utensils and the exercise of great care in the sampling, sub-
sampling, compositing and preserving.

In the beet industry the polarization is practically the true
sucrose (with rafifinose absent) while in the cane industry the
polarization is never the true sucrose but is the algebraic sum of
the several optical activities, of all the participating bodies, not
removable by lead acetate. Therefore, in this article the term
polarization or "sugar" signifies the polariscopic reading when
reduced to terms of '26 grams of material in 100 metric cubic
centimeters. Sucrose, refers to the Clerget figure.

A few terms peculiar to the cane industry, may well be defined
here.

Normal Juice. Strictly speaking this is the whole juice of the
cane as it exists in the tissues, or the combined juice of all the
mill units when milling without the application of water of satu-
ration. It still has considerable significance in cane work but none
in the beet. It usually runs from o.i to 0.7 degree Brix lower
than the so-called First Mill Juice; it is also lower in purity.
Owing to its variability under changing conditions' it should be
determined by actual run, without water, at stated intervals.

It does not appear that a proper figure can be obtained in less
than y2 hour's run. Its Brix, taken in conjunction with that of
the mill raw juice, is used in calculating the extent of the dilution
due to the water of saturation.

Mill Extraction. The percentage of the sugar in the cane that
has been removed by the milling process.

Retention. The amount of sugar in the form of commercial
sugar, expressed in terms of percentage of the sugar obtained in
the milling process.

Total Efficiency. The total sugar in the form of commercial
sugar expressed in terms of percentage of the sugar in the cane.
It is the product obtained by multiplying the extraction by the
retention.

Blanc. A product of vacuum-pan boiling upon very low prod-
ucts variously termed "filete" and "string-proof." It is not boiled
to grain, but is made very concentrated and the density judged

222 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

by pulling a small quantity out to form a "string" or rolling a
small ball in cold water and noting the hardness.

It is the final boiling in all houses not provided with crystal-
lizers, the product being set aside in storage for slow cooling and
crystallization, for from two to three weeks or more.

A very brief account of the processes of sugar manufacture
may assist in making clear the purpose of chemical control and
scheme of sugar accounting. United States beet and Cuban raw
sugars only are considered.

Beet Sug.\r.

The factories of the United States make standard white granu-
lated sugar in one operation from the sugar beet, which has a sugar
content of from 14 per cent to 23 per cent average for the entire
crop or "campaign," according to territory, season and seed
pedigree.

1. Diffusion Juice. The beets are washed and then sliced into
strips 3,'/2 to 7 mm. wide and 2-4 mm. thick, with cross-section
V-shaped and the sugar extracted by a highly developed process
of diffusion, at definite temperatures, leaving behind the "pulp,"
of sugar content 0.25-0.30 per cent. There results a very clean,
but dark colored liquor, warm to hot, of density 0.8-0.9 that of the
original juice of the cossettes (sliced beets), which goes to duplicate
tanks for measurement, after which it is forced by centrifugal
pumps to tall, closed tanks.

2. Liming and Carbonitatioii. Lime to the extent of 2].'^ per
cent to 3 per cent of the beets or lime-saccharate as pro-
duced, both in the form of "milk" of 17° Be., is added, while
simultaneously the mass is brought to a definite, high temperature
by injected steam and carbonic acid from the lime kilns is pumped
in. At the precise moment of granulation of the precipitate of
CaCOj, etc., judged wholly by the eye and corresponding to
0.1-0.14 per cent CaO alkalinity, the mass is released to the
pumps which serve the set No. i filter presses.

3. The Filtrations. After issuing from the first set of presses
under 2^ atmospheres of pressure in form of a brilliant, pale
straw-colored liquor, it goes to a second set of tanks for further
liming and carbonitation, where the alkalinity is brought to 0.015-
0.025 P^'' '^•^"t CaO. It is then passed through a second set of filter

CHEMICAL CONTROL IN SUGAR MANUFACTURE 223

presses and then "sulphured." The presses are clothed with duck
or jute or both. The press cakes are washed with hot water
(condensed) to a definite sugar content, set No. i to i per cent,
set No. 2 to 0.5 per cent, judged by applying a suitable hydrometer
to the issuing "sweet waters."

4. "Sulphur Station" No. i. Bleaching by means of SO., gas
takes place here, reducing the reaction to faint alkalinity, neutrality
or faint acidity as occasion demands, but always to a definite
figure. The process is perhaps invariably a continuous one.

5. Gravity Filters No. i. Passing through these is preparation
for evaporation under multiple-effect system.

6. Concentration. By means of quadruple or quintuple effect
the density is raised to 60° Brix, some ammonia is given ofT, lower-
ing of alkalinity in the absolute but rising as result of concentra-
tion ; some precipitate forms. "Thick juice" results.

The work is now in the "boiling" house.

7. "Sulphur Station" No. 2, or "Bloiv-ups." The reaction is
here brought to the desired point, either faintly alkaline or acid
and by careful test, in accordance with a figure that has been
found to give the best results at that factory and particular district
and often influenced by the season: 0.02 per cent CaO (basis) is
seldom exceeded either way. Acidity may be aided by phosphoric
acid ; alkalinity induced by lime or soda ash. The thick juice, like
all products passing this station, is here "blown up" with injected
steam and reduced to uniform Brix, quite generally 60°, to dis-
solve any grain, aid filtration and promote good boiling in the
pan.

8. Grazity Filters No. 2. These serve all products in the
intricate but systematic work of the "boiling" house such as thick
juice, high and low wash and greens and melted sugar, removing
all suspended matter in preparation for the pan-service tanks.

9. The Massccuitc. This is formed in a vacuum pan working
under 26-28 inches of vacuum and in masses of many tons.

The boiling to grain is carried out purely as an art by men
who make it a profession. Of course, it is based entirely upon
well-known scientific principles. It is essentially crystallization-
in-motion, during which the product, constantly augmented in
quantity by fresh injections of liquor, is resolved into grains of
sugar and a more or less de-sugared mother lic|uor.

224 AM ERICA. \ INSTITUTE OF CHEMICAL ENGINEERS

The (inal result of tlie process is judged upon tlie so-called
purity test. The initial product from the beets generally carries a
purity of 88; as the sugar crystallizes and is removed by the
centrifugals the purity ratio necessarily lowers, thus becoming a
measure of efficiency and of paranx)unt importance.

The first boiling, followed by hot turbinating, gives, upon wash-
ing or "covering" with diluted liquors, white refined sugar, a "wash"
of 90-92 purity and a mother liquor of 78-80 purity. A second
boiling to grain, massecuite having 78-80 purity, discharging while
hot to the crystallizers, cooling there with the aid of a heli.x and
water jacket for about 3 days and then ccntrifugating, gives a
yellow sugar and an exhausted molasses, purity 58-60. The yellow
sugar is redissolved and boiled, variously combined, to white refined
sugar.

If it is the intention to recover still more sugar from the
molasses so reduced in purity that it will yield no more sugar by
crystallization, the sugar may be precipitated by a large excess of
one of the oxids of the alkaline earths.

In the United States lime oxid is used, in absolutely anhydrous
and impalpable powder. Tricalcium saccharate results, later soluble
in the saccharine juice to monocalcium saccharate.

10. The Coolers. Under agitation the powdered lime is slowly
sifted into the molasses previously reduced to 12-14° Brix, kept
cool at a definite temperature meanwhile, until the density of a
filtered sample indicates 6-7° Brix. It is then filter-pressed as
quickly as possible.

11. Saccharate Presses. The ordinary Kroog type of press
produces 40 cakes of i inch thickness ; the saccharate presses
produce a much thicker cake, usually 2'/- inches thick ; they fill
and wash readily. The product from the coolers is here separated
into the saccharate of 86-98 purity and a mother liquor known
as "press waste water" of 6-7° Brix and 10-20° purity, all from
a 58-62° purity molasses. The w-ashing with cold water alone
or combined wMth its own higher "sweet waters" is continued until
a liquor having a Brix of 2^ to 3° results and the purity of the
last runnings mounts to 15-30. The total product of the washing
is known as "wash water."

12. Saccharate and Saccharate .^filh. The saccharate press
cake is transported to the liming and carbonating station of the

CHEMICAL CONTROL IN SUGAR MANUFACTURE 225

main factory process, in the form of milk, being discharged directly
into tanks provided with stirrers, where it is incorporated with
liquors brought thither from various parts of the factory and bear-
ing from known small amounts of sugar to mere traces.

A separate sugar account is required for the saccharate process
and the yield should be about 67 per cent of the sugar charged
to it, in the form of refined white.

Cane Sugar.

Raw sugar factories dealing with cane aim to produce a sugar
that will keep during storage and transportation, of a sugar con-
tent that will bring the highest price for the total sugar output
and to get as high a yield as can be proved to be economical in the
final summing up of all the conditions.

It is generally conceded that an even 96° Ventzke polarization at
the port of entry brings the highest profit. It is very probable that
all other grades will soon be suppressed.

I. The Mining. Heavy iron mills replace the diffusion battery
of the beet-sugar process. The installation generally consists of
three units (individual mills) placed in tandem and composed of
three rolls each ; there are intervening conveyors and the whole
train is preceded by a crusher of two rolls.

The crusher serves to break the outer rind and the nodes, liberat-
ing at the same time considerable juice which flows to the bed plate
of the first vmit. The rolls are ponderous; 7 feet long by 3 feet
in diameter may be taken as a type.

The cane gets two compressions in passing through each unit,
being sustained by the "turn bar" as it issues from between the
cane roll and the top roll and passed on to be caught by the bagasse
roll and the top roll for the still closer compression.

The cane, not being laden with molasses-forming salts to the
great extent that the beet is, the rupture of the cells is not attended
with disastrous consequences. Naturally the ratio between the fiber
of the cane entering any given unit of the tandem and that of the
bagasse issuing therefrom, is a measure of the efficiency with respect
to the amount of liquid expressed. Where water of saturation is
applied, hot or cold, it is generally sprayed forcibly upon the bagasse
as it issues from the unit next the last, at the point of immediate

226 AM ERIC A If JSSTITUTE OP CHEMICAL ESGI. SEERS

release from pressure ; the imbibition of the thin juices is the further
development of the water treatment and is simple and effective.
As high as five units and a crusher or in all, seventeen rolls have
been employed in one tandem.

The juices from the first and second units only enter the process
of manufacture, i. e., under a system of combined saturation and
imbibition, and, united, constitute the mill raw juice.

2. Mill Raiv Juice. Sometimes called diluted juice.

With respect to its purity it is considered to represent the original
juice of the tissues of the cane.

It is either at factory temperature or a trifle above it, depending
upon the saturation water temperature; it is charged with air, turbid
from suspended albuminous matter, wax, insoluble salts, clay, and
fiber — this even after being strained through copper or brass sieves
of 15-19 perforations per linear inch.

It is pumped to tanks for measurements or weighing and is then
■ limed. Where heavy liming with carbonitation is not practised
(and I know of no factory in Cuba doing this) the juice is only
neutralized.

3. Liming or "Tempering'' the Juice. This is generally accom-
plished in sets of three large tanks per tandem, one filling, one under
treatment and one discharging. Repeated trials upon different
sized tanks have shown a size corresponding to three hectoliters per
ton of cane per hour to be advantageous.

Chemists carry the reaction of the juice generally about neutral
to litmus paper. The subject can be said to have been scarcely
attacked from the quantitative standpoint.

Continuous liming is practised in some factories.

Lime and heat form clear juice and cachaza or "scum."

After liming, the juice is passed through heaters where the
product may be even superheated if <lesired, depending upon whether
it is desired to eliminate all the air by a "flashing" operation before
complete settling. If the air is not eliminated a thick scum rises
to the top at 95° C. called "blanket," a small portion sinks to the
bottom, while the separation is being effected in so-called defecators
varying in size from 35-100 hectoliters, net; the time for making
one complete round of the defecators will be 60 minutes but capacity
should be had for 90 minutes, to allow for irregular liming: 15 per
cent of the time will be consumed in filling, emptying and cleaning.

CHEMICAL CONTROL IN SUGAR MANUFACTURE 227

Continuous settling is effectetl in the Deming process and in the
Hatton defecators.

The sHghtly opalescent, straw-colored juice is generall)' run,
without filtration, merely decantation continuous or interrupted,
directly to the multiple effect.

It should be passed through fiber or gravity filters if for nothing
more than to catch much cachaza that slips into the process inter-
mittently. The decanted cachaza is washed by decantation in small
tanks and then sent to frame presses for compression and sometimes
washing. Evaporation is carried to 55° Brix in a cane house, to
facilitate ( i ) settling and ( 2 ) avoidance of false grain.

The boiling of the meladura to grained massecuite is similar in
principle to that carried out in a beet factory.

Cane products grain with great facility, while beet products some-
times present great difficulty, conditions brought about by the vari-
ance in the character of the non-sugars, purity remaining the same.

Generally three grades of grained massecuites are boiled where
crystallizers have been installed, all upon a nucleus of original
meladura which ranges in purity from 80-92, according to district
and time of season. First massecuite, purity 80-84, yielding a sugar
polarizing 97-98° Ventzke and a corresponding green syrup or
molasses of purity 60-64. Second massecuite, purity, 70-74; cor-
responding molasses, centrifugated hot, 48-54; centrifugated after
limited cooling in motion, purity 40-46 ; resulting sugar, washed by
water or liquors to 96° V. Third massecuite, purity 58-63; cor-
responding molasses (final product), purity 30-35; resulting sugar
polarization depending upon treatment. This last massecuite, when
at 35-40° C. and 4-5 days old in crystallizers, is generally centrifu-
gated and the untreated sugar discharged into a mixer where high-
grade molasses is incorporated with it and it is again centrifugated
and washed to the degree -desired, generally 96. This process is
styled "mingling."

In factories not provided with crystallizers (which keep the grain
in motion) the exhaustion of the product when it reaches the purity
48-54 must be accomplished "at rest," which is brought about by
discharging the final boiling, boiled "blanc" to a Brix of from 88-91.
according to conditions, into small iron wagons or into large tanks
where it is allowed to cool quietly and crystallize spontaneously for
from 12-21 days or longer.

228

AMERICAS INSTITUTE 01- CUEMICAL ENGINEERS

The Control

SAMPLING AND ANALYSIS

The Cane. Determine fiber and sugar once each factory day.

Sampling. Every hour, four representative canes are to be
selected under the chemist's supervision, as they pass from cars,
wagons or hopper to the first unit of the tandem. Reserve in a cool,
shaded place. If the factory runs six hours or less, prepare the
whole sample; if more, subsample to 24 canes as follows: Sort
into three piles, one containing the pieces bearing evidence of having
been cut in the fields next to the root ; one, pieces cut from the

Fig. I. — Hopper for
Chopping Cane.

Fic. 2. — Continuous
E.xtractor.

middle ; one, pieces bearing base of the "cogollo" or top of the cane.
Take, impartially, eight pieces from each pile and cut into transverse
slices 5^-1/16 inch thick by means of a Pellet cane cutter, feeding
the tops to the machine first and rejecting no odd ends. Allow the
slices to fall into a galvanized iron box large enough to hold the
entire sample ; throw upon a large, clean piece of enameled cloth,
mix well and quickly subsample by "coning and leveling" until about
a liter is obtained: weigh this carefully. Chop in a hopper (see
Fig. I ) resting upon a clean piece of enameled cloth, with a heavy

CHEMICAL CONTROL /.V SUGAR MANUFACTURE 229'

cane knife (calaboso) when finished, brush up all pieces that may
have fallen upon the cloth and again weigh.

Correct for loss by drying out during chopping. Hopper must
be employed for cane exclusively.

Sugar Determination. Lightly pack 52 grams in a continuous
extractor^ and slowly pour through the mass sufficient 40 per cent
alcohol to fill the 4-oz. Adam's flask two thirds full ; maintain the
flask contents faintly alkaline with basic lead acetate; extract for
three-fourths hour or for such time as experience shows, under
working conditions, is sufficient to extract the sugar to 0.05 per cent
limit using a perforated asbestos plate and low flame. Place the flask
upon the water bath and expel the alcohol ; rinse into a 100 cc.
flask, add sufficient basic lead acetate, fill to the mark, filter and
polarize. Reading divided by 2 equals sugar.

Fiber Determination. Lightly pack 52 grams in the continuous
extractor, allow cool or tepid water to run slowly through during
1-2 hours ; then, slowly, about a liter of water heated to 60° C. ;
connect the flask containing 40 per cent alcohol and extract for
three-fourths hour ; withdraw dregs by means of the rod attached
to the bottom sieve diaphragm to a drying dish ; dry for 2-4
hours to constant weight at 105-110° C. Calculate fiber. To dry
cane or bagasse fiber, employ shallow oblong tin trays, 4" by 5"
and i^" deep, bottom consisting of copper cloth of 80-100 meshes
per linear inch.

The B.^gasse. Sugar may be determined every 2 hours, fiber
once a factory day. Well ground bagasse (modern milling) niay
be taken by the handful as it rises from the mill-boot of the
discharge conveyor and tightly pressed into the sample can, which
may be 2 feet deep by i foot diameter. Fifteen minutes intermit-
tent sampling should fill the can and there should be the minimum
delay in preparation for analysis.

Coarse bagasse (such as that of the first, second or even third

^ This extractor is made of nickeled copper and is very durable ;

vapor pipe insulated, thus promoting rapid exhaustion of contents besides

serving as a handle ; it is suitable for use with cossettes, "pulp," drug and

material of many kinds calling for restricted quantity of solvent.

Especially designed to eliminate "bumping" entirely. An easily remov-
able screen diaphragm retains the material in place, which, after extraction,
may be quantitatively removed for drying and weighing. Made by Eimer
& Amend, New York. Standard size 11 cubic inches net capacity.

230

/1.U£^/C.1A' ISSTITITE OF CHEMICAL EXCIXEERS

unit of the tandem on old-style milling) should be taken from its
particular conveyor, clear across the blanket and amount to at
least i^ cu. ft. in volume.

Throw the can contents to the floor upon a large sheet of
enamelled cloth, tearing coarse pieces apart by hand. If still warm
(hot saturation) cover lightly with a second sheet of cloth for a

Fig. 3. — Bagasse Cutting Machine.

few minutes. Rapidly mi.\ by stirring and rolling, exposing the
minimum surface and pile in a cone; level from the apex outward
to a truncated cone and withdraw a wedge-shaped sample, in size
proportionate to the coarseness of the bagasse. Cut up the whole
sample and mix. A fully satisfactory machine for quickly reducing
large amounts of bagasse to fine "sawdust." is that made by Boot
and Krantz, The Hague, Holland. See Fig. 3.

CHEMICAL CONTROL IN SUGAR MANUFACTURE 231

Polarization. This is performed as under cane, with the alka-
linity maintained with a 5 per cent solution Na2C03.

fiber Determination. This necessitates a very finely divided
material. The Hawaiian Sugar Chemists' Association defines fiber
as "the total insoluble solids," water being the solvent.

Quantitatively remove the residue left after extraction of the
sugar to a drying tray and dry for about an hour, then transfer to a
large, loosely covered container; do this on every sample of the
factory day. At the close of the day there should be, in the container,
the practically dry residues of 12 normal weights. Mix well, weigh
the accumulated samples, take one-twelfth, place in a drying tray
and dry for 2-t, hours or to constant weight. Divide the weight
by 26, multiply by 100, result is percentage fiber in bagasse.

If 10 samples only have been extracted, take one-tenth, etc.

Alternate Sugar Method. Use that as adopted by the Hawaiian
Chemists' Association, 1910, Bull. ■},2, Agricultural and Chemical
Series, Experiment Station, Hawaiian Sugar Planters' Association,
by W. S. Norris.

Moisture. As this serves to judge of the tax laid upon the
furnaces by reason of the water to be evaporated ; calculate by
"difference."

Mill Rav/ Juice corresponds to the diffusion juice of the beet
industry. It is the main basis of sugar accounting and great pains
should be taken to make it fully representative of the work.

Sampling. The following method by means of a thin, rapidly-
running stream has been found to be representative.

Modern mills, in general, discharge the mill raw juice from the
free end of a pipe into a small reserve or over-flow tank, which in
turn serves the measuring or weighing tanks proper.

At a point a short distance below the level of the discharge
(in order to secure a slight "head") the main discharge pipe is
tapped by a half-inch pipe in such a manner that a small quantity
of juice continuously finds the way to its destination, the reserve
tank, through it. A small copper wire, preferably not over 4 inches
long, may now be attached to the end of the half-inch pipe and
a thin stream of juice diverted so as to discharge through a hole
in the side of a covered, 2-gallon pail. Another location for this
half-inch pipe, not quite so advantageous, is in the same main
raw juice line but close to the pump, returning the diverted

232 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

|,ortion of juice to llie pump-lank and interposing the copper wire
in the stream, as described. This latter arrangement reduces the
])ump efficiency about i per cent in a looo-ton factory. The ha'f-
incli pipe should have but one cock, and that next the open end,
to allow for closing when the pump is not operating.

The collection of sam])les is apt to be a weak point, on account
of jjlacing too much reliance upon a messenger. It should be
reduced to a simple system, proper conveniences supplied, and
closely supervised.

In tropical work, evaporation is rapid and the air is full of
spores. All samples should be removed from the factory at fre-
quent intervals and let the chemist either analyze them at once
or properly preserve them. The messenger may collect the follow-
ing samples every two hours. Mill raw juice, first mill juice, last
mill juice, residual juice, evaporator thin juice and mcladura.
Assuming that these are already discharging into their containers
there will be needed for substitution six other clean and dry
sample pails containing sufficient formaline. Not all of the
sample collected can be or should be taken to the laboratory —
after mixing, the greater bulk will be at once returned to the
process of manufacture. For this purpose, separate clean and
dry metal paddles will be needed for stirring. A tray of light
material holding six, liter Mason jars, plainly labelled and with
screw tops will be needed for receiving the sub-samples.

Analysis. Strain the sample into a clean, well-rinsed Mason
jar and let stand until the foam has risen ; carefully remove the
same with a teaspoon.

A. The Brix. Slowly fill a tall cylinder by pouring down
the side; carefully insert the hydrometer, let stand until it has
come to permanent rest, then read and note the temperature ;
correct for hydrometer error, if any and to standard temperature.

B. The Polarization. Slowly fill a loo-iio cc. flask to lower
mark, clearing up any uncertain meniscus with a drop of ether,
run in the prescribed amount of basic lead acetate and fill to the
upper mark with water; shake thoroughly, filter and polarize,
employing the Schmitz table for sugar percentage. If the analyses
must be made at longer intervals, composite as follows: Prepare
as above for "A" and "B:" instead of proceeding with "A," pour
200 cc. into the compositing jar containing the proper amount of

CHEMICAL CONTROL IN SUGAR MANUFACTURE 233

formaline; for Brix: proceed with "B" as far as filtration, then

pour the whole contents of the flask into the compositing jar for

polarization.

When making the determination, thoroughly mix the contents

of each compositing jar, proceeding as under "A" for Brix. Filter.

polarize and consult Schmitz's table for sugar percentage.

C. Set aside in a suitable jar a portion of the unliltered

"leaded" solution for the daily composite determination of sucrose

by the Herzfeld-CIerget method and invert sugar.

When making these last two determinations, add sufficient

acetic acid to transform all basic lead acetate into neutral or slightly

acid condition, correcting for increased volume in final calculation.
First Mill Juice. Sampling. This must be representative of

juices coming from combined crusher and first unit of the tandem.

There is no agreement in either Brix or sugar

content nor in the quantity of the juices falling

from (i) the crusher, (2) the cane roll, (3)

the bagasse roll ; hence the logical place for

continuously and systematically drawing this

sample is in the trough conveying it to the mill

raw juice pump. Fig. 4 shows a successful
Fig. 4.— Juice Sampler. . • r ^ 1 ■ ^1 ■ 11

device tor takmg this sample.

An objection to this will sometimes be that water used to cool
the mill bearings finds its way into this sample, the effect being to
raise the figure for extraction.

The trough sample then becomes useless and a second sample
should be taken by placing a suitable pail beneath the cane roll of
the first unit at a point where tests show that the Brix and sugar
content correspond to those of the trough sample when not con-
taminated by water. This pail holds about 8 liters and has a cover
slightly inclined ; holes are made near its apex, from the inside
outward, sufficient in number to about half fill the pail in 2 hours.

Analyze as under mill raw juice, "A" and "B" only.

Third Mill Juice. The sample, where saturation is practised,

1 The "spoon" sampler consists of a large spoon having a hollow handle
of copper communicating with a hollow shaft of small piping and discharging
through an elbow into a pail charged with formaline. The shaft, driven
from the mill-roll should make about 8 r. p. m. The spoon is covered with
fine screen to keep out "trash."

234 AMERICAS IXSTITUTE OF CHEMICAL E.\CI.\EERS

is taken from its pump discharge pipe as described under mill
raw juice. Where it is not, the spoon sample may be used in
the trough. For analysis, see under mill raw juice, A and B only.

Ri:siDUAL Juice. This is the drij) from the bagasse roll of the
last unit of the tandem and should be taken continuously, as under
first mill juice and analyzed as under raw mill juice, "A"' and "B."

EvAPOK-vroR Thick Juice. The Brix of each tank tilled should
be taken. Where fluctuation in purity is considerable, as between
/O and 85 for instance, facilities should be at hand for rapid
determination of purity. For this 'and similar work the author
has introduced the Pellet continuous polarizing tube.

Filter Press Cake. The loss from this source is seldom
correctly determined. At reasonable intervals the laboratory mes-
senger should go to the trucks located below the presses and as a
press is dumped, break off small pieces from a dozen large cakes;
if semi-fluid a cup should be used. Analyze in the usual way but
substitute 25 grams for a normal weight to allow for insoluble
material. Periodically the weight of the press cakes should be
determined.

The Sugars. Large centrales employ fans for cooling and
rendering the sugar more uniform. Where not used, the net
weight per sack must be verified when cold and finally loaded.
The weight is still held by custom at 325 Spanish pounds of 460
grams each.

Sampling. A clean and dry galvanized iron bo.x of about i
cu. ft. capacity and having a funnel-shaped hopper in the cover,
is placed at the sugar scales, to be changed once every 6 hours.

From every bag in five, and before adjusting the weight with
sugar from the storage bin, the truckman will transfer a pinch
of sugar from bag to sample box. As the sample is taken away,
the serial number of bags filled will be recorded, in order to arrive
at the number of bags represented, in proportion to which the
polarization is to be adjusted in taking off averages.

Preparation. The sugar is poured upon a plate of glass, all
sticks and foreign matter removed and thoroughly mixed with a
clean steel spatula. Lumps are reduced with a porcelain roller
and incorporated with the rest of the sample. Polarize at once.
Determine moisture once a day. Composite a small portion from
each sample for the semi-monthly chemical statement upon which is

CHEMICAL CONTROL IN SUGAR MANUFACTURE 235

to be determined, (i) polarization, (2) true sucrose, (3) dry
substance, net (4) invert sugar (5) ash, (6) total dirt, (7) ash
in total dirt.

When the sugar contains over i per cent moisture, the sample
for compositing is to be dried in a water-bath oven for a short
time, later correcting the final analytical data back to the basis
of the average of the daily polarizations upon the fresh sample.

Polarisation. A normal weight is placed in a funnel and
washed into a 100 cc. flask with 50 cc. of water, completely dissolved
by rotating, then clarified by lead-^-acetate solution and 2 cc. of
alumina cream. As a rule not over i cc. of lead solution is needed
for high-grade centrifugal (96) sugars and from 2-6 cc. for
molasses sugars (80-90). Use the minimum quantity necessary
for clarification. After the lead and cream are in, allow air bubbles
to rise and complete volume to 100 cc. Mix and filter in a carefully
covered funnel, discarding the first runnings. Endeavor to polarize
at the temperature of dilution.

The Massecuite. Applicable to either grained or blanc strikes.

Measuring. Massecuite intended for the crystallizers should
be measured after being placed therein, at the moment of enter-
ing and for every strike, the same applies to sugar wagons or tanks.
The volume of material subject to crystallization jn motion for
long or short periods or "at rest" for many days, should be known,
as an important step in control.

An accurate account should be kept of the movement in and
out, so that at any time, by consulting the records, a balance can
be struck of the exact amount in stock.

Sampling. Take a portion equal to 2 liters from at least three
places as the mass is struck from the vacuum pans, viz., after it
is running well, in the middle of the flow and toward the end.

Analysis. At the laboratory the following tests are made.
(i)Purity of the mother liquor, (2) brix by double dilution. {3)
polarization.

Purity of the iMothcr Liquor. Grained massecuite only. Inves-
tigations upon the work of competent sugar boilers has shown
that this test has a very important bearing upon economical boiling.
The drop in purity may be very variable for equal purity of strike.
Immediately after being drawn the sample is to be rapidly turbin-
ated in the small laboratory centrifugal.

236 AMERICAN IS'STITUTE OF CHEMICAL ENGISEERS

The author has devised special, hght-weight, tin hnings for the
centrifugal; these can be kept on hand in any
number, they slip in and out easily, collect the

^CZa

whole sample and do away with the necessity
of cleaning the centrifugal. It is especially
helpful in making a large number of such
analyses.

When the lowering of purity is abnormal,
either way, the several causes to which it
may be due should be investigated. The purity F"'- 5-'<«;moval)le

, ■ , r. 1-1 .• i o on- Cciitnlugal Lining.

IS determmed after diluting to 18-20 IJrix.

Polarization. This is made by taking either a normal or double-
normal weight of the sample used for determining the Bri.x by
double dilution, according to color, and proceeding as under the
sugar, polarization, excepting that after filtration the solution must
be acidulated before reading, viz. :

Fill a 50-55 cc. flask to the 50 cc. mark with the clear filtrate,
add dilute acetic acid to faint acidity and complete to the 55 cc.
mark with water ; shake and polarize ; increase the reading by one-
tentli to compensate for the dilution.

W'iieii possible, clarify with neutral lead acetate and thus avoid
later dilution.

Ei-FiciENCv OF Crv.stai.lizers. This refers also to work carried
on "at rest" in tanks or wagons. The mother litjuor is separated
by the laboratory centrifugal and its purity determined at 18-20°
Brix, when the product is about half discharged from the vessel.

FiN.XL MoL.\ssES. This should invariably be weighed, being
too viscid to measure and occluding much air.

Under a suitable arrangement one man can attend to the day's
output. The well mixed day's composite sample is analyzed for,
Brix by double dilution, sugar and purity (calculated).

Daily, a quantity in proportion to the amount made is set aside
for the semi-monthly complete analysis, as detailed under sugar.

Control of the Boiling. Much can be accomplished at the pan-
service tanks to bring about regulated, economical boiling. If they
are uniform in size, deep, rather vhan broad, large rather than small
and with facilities for rapid and thorough cleaning, much will
have been gained. The several molasses are diluted to an exact
Brix, generally 60° and heated to 70° C. at a "blow-up" station

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

237

over these tanks. Every tank and piece of apparatus in the fac-
tory should bear a number. These tanks should be graduated to
lo hectoliter units, vertically, upon a scale having an indicator
actuated by a float.

Before the contents of a tank is started for feeding the vacuum
pan the following data concerning the material are to be entered
upon the sugar-boilers blackboard : Date, hour, tank number, name
of material, temperature, Brix, and where possible, the purity.

Upon the basis of this data the massecuite purity is established
and the finished product should agree within two points of the
estimated.

Weights and Measures as Affecting Mill Extraction.
( I ) The Sugar Cane is bought by the Spanish ton as a matter of
tradition. From the time it enters the factory the metric system
should apply. It suffers variable shrinkage in weight before it is
ground and proper chemical control has necessitated the present
policy of weighing it upon a beam scale at the hoist just before
discharging into the mill hopper.

(2) The Mill Razu Juice is generally measured
and when properly carried out, this will furnish
a basis of calculation for the amount of sugar
introduced (the real object) quite as satisfactory
as weighing. Foam and occluded air have been
the cause of some agitation in favor of weighing
the juice, but this entails considerable expense
that the author does not consider always justified.
The installation of measuring tanks on the
capacity basis of 3 hectoliters net per ton of
cane per hour (i. e., 150 hectoliters, net for 1200
tons daily capacity) eliminates occluded air to
a negligible quantity, while a float of special
size and shape enables the true level of the juice
to be determined with exactness and simplicity.
This is shown in Fig. 6. It is made of gal-
vanized iron, conical at both ends, weighted
with gyi lbs. of lead and provided at the top
with a tube 2 inches long for holding a very light rod of wood,
which in turn bears a double arrow and which is brought to a
fixed point upon a scale.

Fig. 6.— Float.

238 A.MEKJCA.\ INSTITUTE OF CHEMICAL ESCl SEERS

Tlie point "A"' also serves as a definite spot from which to
gauge the juice level for juices of different densities. The
accompanying table shows the fluctuating juice level with varying
Brix, the tank capacities being calculated accordingly. These levels
are actually determined by floating the instrument in diluted
molasses of juice density in a tall cylinder. The float rises and
fails in a cage. It rests by far for the greater part well below
that part of the juice containing the unliberated air and allows
no air to collect below it. It measures to within one-sixteenth inch
under working conditions.

Brix Reading. Distance A, to Juice Level.
21.3 173 cm.

15.6 15 9 cm-

96 l4.Scm.

4.8 13.2 cm.

The Specific gravity of the juice may be adjusted for varying
temperature by the use of Gerlach's table.

Measuring tanks should be calibrated by weighing water into
them until duplicate weighings agree within the polariscopic error
as determined by the limits of the volumetric method using the
Schmidt table.

(3) Water of Saturation. The average temperature of this
must be known in order to arrive at its weight, as it is probably
always measured. Duplicate tanks serve the purpose of measur-
ing, well, but a good water meter is sufficient, provided simple
means are at hand for occasionally checking it, under actual work-
ing conditions.

(4) The Bagasse. The weight of this, as determined by the
formula, Cane + Saturation Water — Raw Mill Juice = Bagasse,
is fully satisfactory, since the chemical control fails, in any case,
where any one of the quantities is in error.

Stock Taking. The short season requires frequent stock taking
and the author recommends that this be taken once a week until
it has been demonstrated that the factory is working normally,
but after this, with cane work, once a month is sufficient for the
fully detailed report. For this weekly check, advantage should be
taken of a stop and all the products of the factory composited into
one laboratory sample upon the basis of the several volumes, when
one analysis and one calculation will give the desired information.

CHEMICAL CONTROL IN SUGAR MANUFACTURE

239

THE SUGAR ACCOUNT.

All the sugar in the cane must be accounted for and brought
up to a sum total of lOO per cent. The following form is a good
general example.

al Sugar Account.

Sugar in
Cane 100
Per Cent.

Sugar in first sugar

■' ' second sugar ....

" total sugar

' ' press cake

' ' final molasses . . . .

' ' undetermined loss

" mill ra%v juice. . . .

' ' bagasse

' ' cane

78

C7

9

59

88

56

0

5«

10

02

0

84

100

00

4070

494

4565

29

S16

43

5154

446

5600

In a full technical account the above represents about 20 per
cent of the data, the rest including averages of the analyses made of
all the products, together with tons of cane ground, bags of the
various grades of sugar made, time lost for different causes, data
connected with the mill efficiency and the percentage yield of
commercial sugars upon the basis of the cane.

The undetermined loss is due chiefly to the impossibility of
accounting for all material involved in any undertaking.

There is loss from spilling, from inversion, long action of heat
and errors in weights and measures with limits in accuracy of
analyses. When this figure is i per cent of the total sugar in the
juice it indicates good work, when it is 0.5 per cent it is excellent
work.

General Methods.

Brix by the Hydrometer. All solutions up to 70° Brix are
to be tested by the hydrometer directly, after the removal of air
bubbles.

If the reading is not made at either 175^° C. or 20° C. correc-
tions will be made by means of tables to be found in any standard
te.xt-book.

240 AMERICAN INSTITUTE OF CHEMICAL ENCIXEERS

DounLE Dilution Method. (For products of over 70; Brix.)
— The absence of cold water in tropical work precludes the cooling
of solutions that have once been heated. The following method has
been found most practicable: Use nickel plated, copper beakers
of such size that the fist may readily be introduced. Select two
of about equal weight and place upon opposite pans of the balance;
from the heavier, file or cut off the material around the upper edge
until they exactly balance. With the beakers now upon opposite
pans of the balance, in one place about 400 grams or any conven-
ient quantity of the material ; into the other pour water until exact
balance is secured ; remove the beakers from the balance and pour
the water of the one into the other containing the material ; by
means of the hand, mix the two until the last grain is dissolved, do
not remove the hand until the operation is complete, in fact,
endeavor to keep the hand equally submerged all the time.

Allow to stand until air has risen, take the Hrix by the hydrom-
'eter, correct to standard temperature and multiply the result
by 2. If the beaker used for water be only lightly greased within,
it will deliver the water to the other to the last drop, thus obviating
pouring back.

The Dilution to 18 to 20 Brix. — For rapid control of the
process of boiling, based upon the purity, all products will be
reduced to uniform density within these limits before making the
test. Simple as it seems, the average chemist is longer in learning
to perform this test with unfailing accuracy than any other test
in sugar manufacture, this being especially true with products con-
taining grain in suspension. The fault lies in losing some of the
material by spilling before all the grain has been dissolved or
before the mixture is absolutely uniform.

( I ) For products positively known to contain no grain.

Select a cylinder 1 5 inches tall by i J/2 inches diameter, having
the upper edge of such a shape that it may be perfectly sealed by
the palm of the hand ; fill about two-thirds with water, pour in
from about 1 10-120 cc. of the material, adding more water until
within about ij/ inch from the top; seal tightly with the palm
of the hand and shake vigorously until mixture is intimate; the
result should always be a solution too dense rather than too thin ;
pour out a portion and add water if trial test .shows too dense,
mixing as before; continue this until i)roper figure is reached.

CHEMICAL CONTROL IN SUGAR MANUFACTURE 241

(2) For products known or suspected to have grain. Select
two-liter enamelled cups of unbroken surface — these have no
corners in which the grain may lodge and thus escape solution.
Pour into the cup about 500 cc. of water, add about 200 cc. of the
material and by means of the hand manipulate the mass until no
more grain can be felt ; transfer the solution to the cylinder and
proceed as under (i) until the density is reduced to 18-20° Brix.

Dry Substance. In the cane sugar industry this is a purely
empirical process and close conformity to certain conditions are
necessary to secure even comparative results. The breaking down
of the levulose molecule at temperatures above 80° C, the oxida-
tion of non-sugars, the formation of acids that in turn produce
more invert sugar which continues to decompose, make it impossible
to dry to constant weight at atmospheric pressure, therefore a
vacuum should be employed, when the temperature is held at 70°
C, the vacuum should not be under 25 inches and a slow current
of dry air allowed to pass through ; weigh every 2-3 hours until
constant in weight.

In the absence of any vacuum the following method may be
used. It is based upon the official method of the Association of
Official Agricultural Chemists, Btill. 107 (revised), U. S. Bureau
of Chemistry, p. 64.

Place in a light crystallizing dish, provided with a watch-glass
cover and stirring rod, 25 grams of broken glass in quite uniform
pieces the size of coarse sand and washed free from dust. Dry
quickly at 120-140° C, cool in a desiccator and weigh. Of sugar,
take 10 grams ; of molasses, 5-6 grams ; of mill raw juice, 35 grams.
Dry for exactly 10 hours at 98-100° C. (boiling water jacket). The
time for drying the juice should begin with the disappearance of
the water.

SuLPH.'VTED Ash. About 3 grams of sugar are used and a
proportionate amount of other products; if moisture exceed 25
per cent, as in cane juice, the water must be evaporated on the
water bath. The true ash is calculated by multiplying by factor
0.9.

Condensed Waters. These include all the main hot water
collectors, the pan and evaporator tail-pipes. To be tested for
sugar with alpha-naphthol. Some form of continuous sampler is
advised.

242 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

The Test. (Fnililing and Sclniltz, .Inlcittoig, p. i66.) To 2
cc. of the suspected li(juid add 5 drops of a 20 per cent alcohfilic,
sugar free, alpha-iiaplitliol solution, then 10 cc. of purest sulphuric
acid and shake thoroughly. With o.i per cent sugar the color is
so deep as pot to be transparent ; with o.oi per cent a bright red
wine.

Boiler Water. Determine the acidity of the boiler- feed water
and the alkalinity of the boiler water every 12 hours.

For the test, take a small amount from each boiler in service,
titrate with standard acid ( i cc. = o.ooi CaO), using methyl orange
as indicator. Report as grams CaO per lOO cc. Report number of
pounds soda-ash used per 24 hrs.

Prep/\r.\tio.\ for Clerckt Test and Invert Sfo.xR. Juiees.
Determine the sp. gr. Clarify 500 cc, strained and air-free with
neutral lead acetate soi. (50° Brix) ; dilute to 550 cc, shake well
and filter. Make the direct reading at as near 20° C. as possible.
To about 150 cc, add ignited Xa^COj to scant phenolphthalcin
alkalinity, stir and let stand 15 minutes; filter. Use exactly 75 cc.
for Clerget by the Herzfeld inversion method. Use about 5 cc.
for invert sugar test.

Molasses. Wash 23/j normals into a 500 cc. flask, clarify
with sol. lead-i>-acetate, mix, rotate to expel air, dilute to the mark
and filter; collect 250 cc, neutralize with glacial acetic acid, double
the amount of acetic acid ; throw the filter and precipitate into the
clear liquor, mix thoroughly and again filter. Polarize and mul-
tiply by 2. Remove the lead with NajCOj and proceed as
under Juices for Clerget Test and Invert Sugar, using 15-20
cc. for the latter. True sucrose should be calculated by the follow-
ing formulae.

Juice Molasses

26 X invert pol. ,. . Direct pol. — invert

— 1 — + direct pol. . , ,

68.18 sp. gr. pol. (2.67)

142.66 — 0.5 t 142.66 — 0.5 /

Hercfeld's Inversion Method. This will be found in detail
in any standard work. After inversion is complete and while still
in the water bath, add i gram powdered zinc, heat for another

CHEMICAL CONTROL IN SUGAR MANUFACTURE

243

5 minutes, pass through cotton, wash the cotton until lOO cc. is
obtained at 20° C.

Invert Sugar Determination. To exactly 10 cc. of Fehling's
solution, blue and 10 cc. of Fehling's solution, white, in a 250 cc.
flask, add the solution under test and enough distilled water to make
50 cc. Boil cautiously upon a square of asbestos, having a central
hole, for 2 minutes, then cool quickly. Add 10 cc. of 20 per cent
solution KI, rotate, add 10 cc. of 25 per cent H2SO4, then titrate
with N/io thiosulphate. Work rapidly throughout, running in by
3-4 drops at the end.

Run a "blanc" upon the Fehling solution, under precise con-
ditions of analysis to determine its value in terms of thiosulphate.
Use the table of MeissP and Hiller to calculate results. Careful
determination by several chemists have shown that not all of the
copper present can be accounted for with cane products and the
following table of factors has been worked out;

Table of Invert Sugar Factors
For use where the copper reduced is determinined bj' difference

Cc. Deci-

Juiceg.

Sugars.

Molasses.

Thiosulphate
Used.

/=±6

/ = ±1.2

/ = ±3.4

/ = ±15

J =±32

/=±39

/ = ±46

J = ±55

5

0.981

0.928

0.950

0.926

0.996

0 934

0.960

0.956

ID

0.998

0.919

0.966

0.961

I. 013

o.gSo

0.983

0.988

IS

1 .007

1. 013

0.989

I. on

1. 017

I. on

0.988

1 .010

iSS

i.ois

20

I .016

1 .048

1 .016

1. 021

1 .020

1.032

1. 001

1 .001

25

I 045

1.03c

0.963

1.022

1.047

1 .002

0.971

Example. Used in "blanc" titration, 27.75 cc, in back titra-
tion, 6.93 cc, net utilized, 20.82 cc. 0.00636 X 20.82 = 0.1324
0.1324

gram Cu,

= 0.0662 = Z. W = 8.275 grams material taken

for determination. Polarization = 10.08. 0.0662 X 100/8.275 =
Y = 0.8 per cent, 100 X 10.08/10.08 -f 0.8 = 92.7 =R. 100 —
92.7 := 7.3 = /. Since 20 cc. of Fehling's solution were used

1 "Spencer's Handbook for Cane Sugar Manufacturers," pp. 129, 130.

244 AM ERICA. \ INSTITUTE OF CHEMICAL ESGI SEERS

instead of 50 cc, Q\\/2 or 0.0662 gram must be multiplief) by 2.5
to find the factor, F., which equals 0.165 gram Cu. By the Meissl
and Hiller table, factor = 53.1. Hence 0.1324 X 53-1/8.275
= 0.85 approximate invert. Referring to the above table of cor-
rections results in that of 1.016. 0.85 per cent X 1.016 gives
0.864 per cent corrected.

Attached will be found a Comprehensive Table cif Purities
arranged by the author for laboratory use.

The Table includes all purities that will occur in natural products
and factory products between Brixes 5 and 30 and Sugars 1 to
28.5 per cent. The Brixes ascend by 2/ioths, the Sugars by i/ioth.
The Purities are arranged in four blocks ; beginning witli the bottom,
first block for sugars i per cent to 5.4 per cent ; second block,
sugars 5.5 per cent to 13. i per cent; third block, sugars 13.2 per
cent to 20.8 per cent ; fourth block, sugars 20.9 per cent to 28.5
per cent.

765 Westminster Road, «

Brooklyn, N. Y.

TABLE OF PURITIES FOR USE IN CANE AND

ARRANGED BY DAVID L. DAVOLL, Ji

FOR USE IN CANE AND BEET SUGAR FACTORIES

ARRANGED BY DAVID L. DAVOLL, Jr.

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COPYRIGHTED, 1913, BY DAVID L. DAVOLL,

This Table of Purities has been arranged especially for laboratory use by the
author. It may be framed in the usual way and the lines followed with a common
ferule, or better, be pasted upon a cylinder 5! inches in diameter made to revolve
upon a vertical axis, one Brix column being cut off and pasted to a fixed edge set
close to the cylinder, when, by simple rotation, any sugar column may be brought
up close to the BrLx column and the purity noted.

The Table includes all purities that will occur in natural products and factory

EXPLANATION OF AND MODE OF USING TABLE OF P

products between Brixes 5 and 30 and Sugars 1 to 28.5%. The BrLxes
2/ioths, the Sugars by i/ioth. The Purities are arranged in four bloi
ning with the bottom, first block for sugars i to 5.4%; second block,
to 13.1%; third block, sugars 13.2 to 20.8%; fourth block, sugars 20.9
If, for instance, the purity corresponding to Brix 238 and sugai
desired, by noting the regularly ascending scale for the sugar per cent

Brixes 5 and 30 and Sugars i to 28.5%. The Brixes ascend by
•s by i/iolh. The Purities arc arranged in four blocks: begin-
:om, first block for sugars i to 5.4%; second block, sugars 5.5
lock sugars 13.2 to 2o.S';t,; fourth block, sugars 20.9 to 28.5%.
:e the purity corresponding to Brix 238 and sugar 18.9% is
the regularly ascending scale for the sugar per cent the figure

1S.9 will be met with in the third block; by now following down the Brix column
at the extreme left, 23.8 will be found; the point of intersection of column under
18.9% sugar and opposite degree Brix 23.8 gives the Purity as 79.4.

Special space has been devoted to purities required for dilutions to 18-20° Brix
in vacuum pan and crystallizer control, the Brix figures being repeated so as to
permit of purity extension to embrace all purities between 30 and 94,

THE ASPHALTIG ROCKS OF THE UNITED STATES
AND THEIR USE IN STREET PAVING

By S. F. PECKHAM

The word rocks in this paper is used in its geological sense, and
comprises all varieties of mineral aggregate that may be saturated
with bitumen. These rocks are found for the most part west of the
Mississippi River. There are deposits of limited extent in Kentucky
and Alabama, but they have not been entered commercially to any
extent.

I was once shown a specimen of bituminous limestone which was
said to be obtained in a quarry in Michigan, but I have never been
able to locate it. The deposits west of the Mississippi River, how-
ever, extend from Utah through Oklahoma and New Mexico into
Texas. They have been worked in Utah and Texas but from an
economical standpoint are almost wholly confined to Oklahoma,
where according to a recent report of the State Geologist, Dr. Gould,
they are of sufficient extent to furnish material for paving all the
cities of the United States.

On a recent trip to the Southwest extending to the Pacific coast,
I had unusual opportunities for learning all the facts that may be
stated in relation to these deposits in Oklahoma and their uses.

Starting from New York on June 9th, I visited first Chicago,
then going south, Memphis, and west to McAlester, Okla. I spent
a month in the vicinity of that city including a side trip to Ardmore,
Okla., where I spent the 4th. of July, and a few days after leaving
McAlester. I spent two days in Ft. Worth, Texas, continuing my
journey to El Paso, thence to Los Angeles where I remained two
weeks, thence north to \'entura where I remained three weeks, then
a week at Nordhoff, thence continuing north to Santa Barbara up
the coast to San Francisco.

Leaving San Francisco by the Union Pacific Railroad, I spent
two days in Salt Lake City, two days in Denver, three days in

245

246 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

Kansas City, one day in Louisville, two days in Washington, thence
returning home to New York.

In all of these cities I took particular pains to observe and
inform myself concerning the condition of the streets, and the extent
to which in each of the cities mentioned so called asphalt pavements
had been used for paving purposes.

The condition of the streets in Chicago might be said to be good
to indifferent. Michigan Avenue which is used largely by auto-
mobiles and which consequently receives a continuous sprinkling of
lubricating oil which keeps the surface of the asphalt soft and
pliable, appears to be in splendid condition, but side streets are more
or less filled with holes and indicate that wrong material was used
although the repairs expended upon them were first-class in
execution.

In McAIestcr, Okla., the asphalt streets were all comparatively
new, having been laid but a few years. They were soft and wavy
in' their surface, easily impressed with the shoes of horses, and in
many instances showed rutting from the action of wheels, all of
which indicate that the materials used were of indifferent value. I
asked a citizen of the city why such streets had been laid when they
had at their doors some of the most valuable materials for street
paving in the world. He replied that the streets were the result of
competitive bidding. The lowest bidder received the contract, upon
which comment is unnecessary.

At Ardmore, Okla., I walked over some magnificent streets,
some of which had been laid five or six years. In several instances
the excessive cold weather of the previous winter had developed
cracks which had not fully closed, but on the whole the streets of
the town which were laid wholly of materials obtained in the neigh-
borhood were in magnificent condition. I asked if any tests had been
applied to those streets other than the wear of farm wagons. I
was told that the corrugated wheels of traction engines some of
which were very heavy made no impression on those streets, and
that the material of Sell's Circus had been unloaded on that particu-
lar street without leaving a scratch behind it.

Proceeding to Ft. Worth. Texas, I was fortunate in receiving an
invitation from a friend to take an automobile ride over some of the
streets of the city. These streets included natural rock asphalt, so
called artificial asphalt and bitulithic surfaces. There was no diffi-

ASPHALTIC ROCKS OF THE UXITED STATES 247

culty in distinguishing these streets by the action of the automobile.
The natural rock asphalt streets were as level as a house floor, the
bitulithic streets were wavy in every surface to such an extent that
in some instances the automobile wheels bounded from one wave
to another. The artificial asphalt streets were in various conditions.

There were two streets that were laid a number of years ago of
the bituminous shell limestone, that occurs at Cline, southwest of
San Antonio, Texas. This shell limestone saturated with bitumen
in its natural condition is exceedingly tough and broken with great
difficulty. After being ground and heated it resolidifies, but as the
shells are broken into small pieces it is only held together by the
bitumen, which becomes quite brittle. The streets laid of this
material had gone to pieces under the wear of heavy traffic and were
in very bad condition.

One of the finest streets in Ft. Worth and indeed one of the
finest I have ever seen is something over a mile in length laid three
years, and is made of a mixture of bituminous sandstone and
bituminous limestone obtained near Ardmore. It was free from
defects of any kind and looks as though those who laid it had
finished their job the day before.

No opportunity was given me to examine any streets in El Paso,
as I stopped there only two hours in the night.

When I reached Los Angeles I was particularly interested to
examine carefully the streets of that city, as I was informed that
$4,000,000 had been expended on streets the previous year. The
centre of the city is well paved, and almost exclusively with asphalt,
the basis of which is obtained from distillation of the petroleum
produced in the neighborhood. The city stands in a region where
the ground never freezes, consequently the heaving due to the
excessive frost appearing in northern climates has never to be
reckoned with. The streets as a general thing present a fine
appearance, but complaints were made by citizens that the surfaces
had to be frequently renewed and were a source of enormous
expense.

Outside the city there are several boulevards which have been
constructed into oiled roads within recent years. They too were
regarded as very expensive in consequence of incessant repairs, and
while the great Sierra ]\Iadre Boulevard was a highway that it was
a pleasure to drive over, the construction of some highways in less

248 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

densely populated sections had proven to be more or less failures on
account of defects due to excessive or insufficient mixture of oil
with soil.

In Ventura County where a few years ago the advent of an oiled
road was hailed with acclamation they were abandoned as im-
practicable for the above reasons. This matter of oiled roads, how-
ever, is a side issue, as they are not strictly speaking asphalt
streets.

In Santa Barbara there are several miles of very fine asphalt
streets. In San Francisco the condition of the streets was very
similar to that of Los Angeles. Presumably the streets in all the
towns of the Pacific Coast are at present laid and repaired with
mixtures made from the residuum of California petroleum. In all
these Pacific Coast towns the newer streets have been laid with
either stone or brick gutters. In some instances the stone was
artificial, in others it was concrete, but whatever the material might
be the gutter was a separate construction from the street, and
received not only a maximum of wear from the action of the
water, but also the drippings of standing automobiles and the
stamping of horses tied to posts. The advantage of this arrangement
was apparent to the most casual observer, for it is well known that
in asphalt street construction gutters have been a serious problem
for many years.

On reaching Salt Lake City the magnificent wide streets of that
place immediately attract attention. Their main streets were, con-
structed in such a manner that with stone gutters and a strip from
four to six feet of Belgian block, the wear of the street from heavy
traffic, from the stamping of horses, etc., was completely removed
from the centre of the street which was laid with asphalt that
received less than one-half of the ordinary wear to which such
streets are subjected. The result was an almost uniform condition
of the streets that was so superior to anything I had seen elsewhere,
that I was ready to exclaim that Salt Lake City had the finest
streets in the whole country. A closer inspection, however, showed
that the material from which these asjjhalt streets were constructed
was soft and not impervious to the influences of the weather. Never-
theless, Salt Lake City has many of the finest asphalt streets that I
have ever seen.

In Denver the streets were narrower, and while thev had

ASPHALTIC ROCKS OF THE UNITED STATES 249

Stone or brick gutters, there were no strips of Belgian block to
receive the heaviest wear of traffic.

I had expected to obtain some interesting items of information
when I reached Kansas City. This city has 200 miles of asphalt
streets in every conceivable condition from almost completely bare
concrete to the finest asphalt street that can be built. I rode over
several streets that had been laid twelve or fifteen years before,
with a mixture of Oklahoma natural bituminous rocks, that had
never been repaired, the most remarkable demonstration of the value
of this material for street paving that I had ever witnessed. One of
these streets in particular, several blocks in length, looked as though
it was not more than a year or two old.

In Louisville, although in the immediate neighborhood of the
deposit of Kentucky bituminous rock, there were almost no asphalt
streets, the main thoroughfares being laid with wood and presenting
a beautiful appearance.

I rode over many miles of asphalt streets in Washington. They
were in magnificent condition as I expected to find them. I observed
that Washington was also laying the gutters of stone or brick. This
is an innovation which is bound to bear good fruit.

Unless the practice in Washington has been changed from what
it was under the administration of Mr. Dow, as is not probable, there
are no streets in Washington which are not constructed of natural
asphalt. By this term, natural asphalt, is not meant natural
asphaltic rocks, but asphalt occurring as deposits of asphaltum in
masses which are afterward mixed with sand and converted into a
street surface. There have never been constructed in Washington
to my knowledge, streets made from natural bituminous rock from
any source. However, for many years, great care has been ex-
ercised in laying and repairing the asphalt streets of this city, the
result of which care has been a general condition of the asphalt
streets superior to that of any other city in the country.

Getting home to New York and Brooklyn, the wretched condition
of our streets was more forcibly impressed upon my mind after
what I had seen. Of course in central New York City, the streets
are subjected to the incessant wear of heavy trafific, but there are
residential streets in New York and Brooklyn, the condition of
which requires the strongest apologies.

One block near where I reside has been laid possibly eight years.

250 a.\h:rica.\ ixsTinTE of chemical exgixeers

but has been repaired every year for the last four years. The
repairs of one season disappeared almost completely. Between
the repairs of that year and the next succeeding one the bitumen
disappeared completely, and the sand blew into the gutters leaving
in many instances the bare concrete. With what material these
repairs were constructed I am unable to say.

These various object lessons observed over such a wide area
and under such varying conditions of climate and commercial con-
siderations that affect the use of materials of different kinds, teach
a very striking and impressive lesson. If streets can be laid, over
which traction engines with their corrugated wheels fail to leave an
impression, and if setting aside heavy traffic, residential streets can
be laid with natural materials that require no repairs for fifteen
years, and if the cheaper materials obtained in the distillation of
petroleum, which are wholly unfit for streets sustaining heavy traffic
do not last on residential streets more than three to five years with-
out repairs, I ask why they should be used, with constant repairs and
renewals when at a somewhat greater first cost materials which are
available, in the long run must prove much more satisfactory and in
reality cheaper in the end.

I have been acquainted with the development of this industry in
all its details in Oklahoma for fifteen years. I was present in 1897
when Mr. C. O. Baxter, as agent of the Gilsonite Paving Co. of
St. Louis, prepared the material in Oklahoma and laid those streets
in Kansas City which have sustained an average amount of traffic
for fifteen years without repairs. I have been informed that soon
after these streets were laid, the Barber Paving Co., purchased the
deposits of bituminous limestone in Oklahoma, and that since then
no work has been done anywhere with the materials then used. It
is a fact, however, that when the proposal was made to the City
Government, in 1908, to use in Ardmore similar materials, a com-
mittee of citizens together witli the City Engineer first experimented
on the proper proportion of bituminous limestone which should be
mixed with bituminous sand or sandstone to form the most satis-
factory materials for paving the streets of that town. They suc-
ceeded after a few months of experimenting in laying a street which
is almost faultless. The work was undertaken by a contractor who
has enlarged his business and improved his methods until the streets
which he lias laid in Tulsa and Ardmore, Okla., and Ft. Worth,

ASPHALTIC ROCKS OF THE UNITED STATES 251

Texas, are unequalled by any similar surfaces anywhere in the
whole country. I was told that the severe cold of last winter gave
them a trial which they had never before received, and that some
of them contracted to such an extent that they cracked.

The party, who constructed these streets, has found that a
softening material, that is really maltha, less fluid than petroleum,
and softer than asphaltum, can be extracted by boiling water from
the deposits of bituminous sand that exist in inexhaustible quantities
twelve miles west of Ardmore.

Summit Avenue, in Ft. Worth, Texas, which represents his last
and most successful achievement in street paving, was laid with a
mixture of bituminous limestone or chalk mixed in proper propor-
tions with bituminous sand, and the whole tempered with this natural
maltha which he has obtained as above described. The result is an
almost perfect street; perhaps it is safe to say that it is perfect,
having been laid three years and no defect can be found in it, not
even a contraction crack, and it is as level as a house floor without
wave 6r buckling, and hard enough to resist rutting even when the
temperature in the sun is above lOO degrees Fahr.

The streets in Kansas City that were laid in 1897 and have
stood ordinary traffic for fifteen years were constructed of similar
materials. It is not claimed that in competitive • bidding these
materials can be furnished at the same price for which a mixture of
sand and petroleum residuum could be laid, but while the first cost
is greater, the average cost for fifteen years is far less.

In the construction of a street the cost of grading is the same
whatever may be the material used for a surface, also the cost of
the concrete foundation. The difference in price relates only to the
surface of the street which is in reality one of the least items in the
total cost of construction.

If there are as Dr. Gould asserts, sufficient deposits of this
material in Oklahoma to pave the whole country, why is such a
problem left out of the calculations of those who have in charge
the construction of streets in our large Eastern cities.

It is well known to those who are familiar with the technology
of asphalt streets, that a certain allowance must always be made
when criticism is indulged on any particular piece of work, for the
skill which has been exercised in the mechanical performance of the
case in hand ; but, such variation in mechanical skill or the lack of

252 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

it, does not explain the difTerencc in results which are evidenced in
the examples set forth in the foregoing relation.

No amount of mechanical skill can convert bad materials into
good streets, nor can a reasonable amount of the lack of it so far
damage the result as to convert first-class materials into poor
streets. This charitable view of the technology of asphalt paving
cannot cover the multitude of sins laid at its door. There is a
fundamental difference in the materials used in this technology and
the sooner that fact is recognized the more rapidly will progress be
made toward the realization of an ideally perfect street, whose good
qualities shall be limited only by their inherent defects ; that is to
say, that a perfect asphalt street as such may not possess all of the
good qualities of an ideally perfect street.

Placing a street made of European Neufchatel bituminous rock
at the head of a list of such structures, the question to be solved
would be, how far all the elements of perfection with which it is
characterized can be realized in any structure made of similar-
materials, or in an imitation thereof.

The solution of this question is brought to the laboratory of
a chemist for a determination of the identity of the materials as the
primary consideration. This determination can be made nowhere
else, for, if under given conditions two substances from different
sources can be made into streets that are apparently identical in
quality, that is no proof of identity in the materials used, nor is it a
warrant that the apparent equality is not accidental.

In the laboratory proximate analysis supplemented by elementary
analysis — no matter how difficult in execution these analyses may
be — can alone determine the identity of the materials. In the years
that have elapsed I have subjected these Oklahoma bitumens to
hundreds of parallel tests with California asphaltum, and with
petroleum residuum. They are not identical, nor are they identical
with Trinidad Pitch or any other South American bitumen that has
been brought to my notice.

These Oklahoma bitumens resemble the bitumens of Seyssel and
Neufchatel more than any other bitumens with which I have com-
pared them. The first and simplest observation is their permanence
under natural exposures to the elements. California asphaltum
decomposes under the atmosphere and disintegrates into a carbo-
naceous soil. Trinidad Pitch with less rapidity does the same thing.

ASPHALTIC ROCKS OF THE UNITED STATES 253

In the latter case the result is a brown pulverulent substance that
assumes prismatic forms. In the case of California asphaltum that
has resulted from the decomposition of the outflows of maltha, the
result of the decomposition is very similar to that of Trinidad
Pitch, but, in the outcrops of veins of asphaltum that occur near
Asphalto in Kern County, Calif., the decomposition proceeds from
the surface downward resulting in a brown substance with rhom-
boidal fracture, resembling carbonate of iron. The outcrops of
Oklahoma bituminous rocks on the surface, though covered with
lichens and having the appearance of long exposure to the elements,
exhibit immediately beneath the surface very little change, if any,
from the conditions found in the interior of the deposit.

When the bitumen is extracted from all of these materials, and
subjected to parallel tests of hardness and flexibility, at low tem-
peratures, it is found that there is no parallelism between these
natural bitumens and the so called artificial bitumens or petroleum
residuums. While those from Oklahoma become more dense, they
remain flexible or at least elastic at zero Fahr. ; while the other
bitumens, either natural or artificial become brittle and fragile. These
facts will explain the difterent results obtained when these different
materials are used for street surfaces. Another simple test, the
result of which is very marked, consists in observing the effect of
boiling water upon the bituminous rock. This test when applied
to Neufchatel and Oklahoma rocks results in a complete separation
of the bitumen from the mineral aggregate. On the contrary when
this test is applied to bituminous rocks from other localities, the
boiling water does not produce any separation.

In the years 1894, '95 and '97, during which I visited California,
and the island of Trinidad, and spent nearly a year in Oklahoma,
I gathered a complete set of specimens, several hundred in the
aggregate, illustrating the points above stated. They embraced
specimens from the Ojai ranch in California, where the decom-
position of asphaltum assumed the appearance of reefs in a sterile
soil that were covered with lichens ; also a complete set illustrating
the decomposition products found at Asphalto ; also a large number
of specimens from deposits of bituminous limestone and bituminous
sand in the vicinity of Ardmore, Okia ; also a complete set of
specimens illustrating the different materials found at the Pitch
Lake in Trinidad.

254 A^fERICA.\ lySTITVTE OF CIVIL ESGISEERS

I lioped for a number of years to be able to make an exhaustive
comparative research on these different forms of natural bitumens,
as well as the artificial residuum from petroleum. I had barely
commenced the work on Trinidad Pitch when the Civil Engineer,
who controlled my work, ordered me to desist. I have published
what little I had accomplished on Trinidad Pitch, but the bulk of the
work remains undone. I have given tlie specimens to the Museum
of the Brooklyn Institute. The work is a work of years and awaits
the labors of a chemist competent to undertake it, who loves chemical
research next to his own soul.

I wish in this connection to express my thanks to Mr. Nelson H.
McCoy, Secretary of the Chamber of Commerce of Ardmore, Okla.,
who has for many years assisted me in numberless ways in my
researches, also to Mr. Clark R. Mandigo, Assistant City Engineer
of Kansas City, Mo., who extended to me in the most courteous
manner every facility for learning the exact condition of the asphalt
streets of Kansas City.

CODE OF ETHICS

Prepared in accordance with a vote of the Institute at the Washington

Meeting and amended at New York Meeting by

Committee on Professional Ethics.

G. W. THOMPSON, Chairman
CHAS. F. McKENNA, A. C. LANGMUIR, A. D. LITTLE

. ARTICLE I.

Purpose of the Code:

To define the rules of professional conduct and ethics for the
members of the Institute.

ARTICLE 11.

The Institute expects of its members :

1st. That in all their relations, they shall be guided by the highest
principles of honor.

2d. The upholding before the public at all times of the dignity of
the chemical profession generally and the reputation of the Institute,
protecting its members from misrepresentation.

3d. Personal helpfulness and fraternity between its members and
toward the profession generally.

4th. The avoidance and discouragement of sensationalism, exag-
geration and unwarranted statements. In making the first publica-
tion concerning inventions or other chemical advances, they should
be made through chemical societies and technical publications.

5th. The refusal to undertake for compensation work which they
believe will be unprofitable to clients without first advising said
clients as to the improbability of successful results.

6th. The upholding of the principle that unreasonably low
charges for professional work tend toward inferior and unreliable

255

25G AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

work, especially if such charges are set at a low figure for adver-
tising purposes.

7th. The refusal to lend their names to any questionable
enterprise.

8th. Conservatism in all estimates, reports, testimony, etc.,
especially in connection with the promotion of business enterprises.
9th. That they shall not engage in any occupation which is obvi-
ously contrary to law or public welfare.

loth. When a chemical engineer undertakes for others work in
connection with which he may make improvements, inventions, plans,
designs or other records, he shall preferably enter into a written
agreement regarding their ownership. In a case where an agreement
is not made or docs not cover a point at issue, the following rules
shall apply :

a — If a chemical engineer uses information which is not com-
mon knowledge or public property, but which he obtains from
a client or employer, any results in the form of plans, designs
or other records shall not be regarded as his property, but the
property of his client or employer.

b — If a chemical engineer uses only his own knowledge or
information or data, which by prior publication or otherwise
are public property, and obtains no chemical engineering data
from a client or employer except performance specifications or
routine information, then the results in the form of inventions,
plans, designs or other records should be regarded as the prop-
erty of the engineer and the client or employer should be entitled
to their use only in the case for which the engineer was retained.
c — All work and results accomplished by the chemical
engineer in the form of inventions, plans, designs or other
records, or outside of the field for which a client or employer
has retained him, should be regarded as the chemical engineer's
property.

d — When a chemical engineer participates in the building of
apparatus from designs supplied him by a client, the designs
remain the property of the client and should not be duplicated
by the engineer nor anyone representing him for others without
express permission.

e — Chemical engineering data or information which a chem-
ical engineer obtains from his client or employer or which he

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS 257

creates as a result of such information must be considered con-
fidential by the engineer; and while he is justified in using such
data or information in his own practice as forming part of his
professional experience, its publication without express per-
mission is improper.

/ — Designs, data, records and notes made by an employee
and referring to his employer's work, should be regarded as his
employer's property.

g — A client does not acquire any exclusive right to plans or
apparatus made or constructed by a consulting chemical engineer
except for the specific case for which they were made.
nth. A chemical engineer cannot honorably accept compensation,
financial or otherwise, from more than one interested party, without
the consent of all parties ; and whether consulting, designing, install-
ing or operating, must not accept compensation directly or indirectly
from parties dealing with his client or employer.

When called upon to decide on the use of inventions, apparatus,
processes, etc., in which he has a financial interest, he should make
his status in the matter clearly understood before engagement.

1 2th. The chemical engineer should endeavor at all times to give
credit for work to those who, so far as his knowledge goes, are the
real authors of such work.

13th. Undignified, sensational or misleading advertising is not
permitted.

14th. Contracts made by chemical engineers should be subject
to the Code of Ethics unless otherwise specified.

ARTICLE III.

For the administration of this Code of Ethics, a Committee on
Ethics shall be appointed by the president holding office at the time
of the adoption of this Code with the approval of the Council, to
consist of five members ; one appointed for five years, another for
four years, another for three years, another for two years, another
for one year, and thereafter, the president then holding office shall
appoint one member annually to serve for five years and also fill such
vacancies as may occur for an unexpired term. All of these
members shall be over forty years of age. The Committee shall
elect its own chairman. The Committee on Ethics shall investigate
all complaints submitted to them bearing upon the professional con-

258 AMERICAN INSTITUTE OF CHEMICAL EXCINEERS

duct of any member, and after a fair opportunity to be heard has
been given to the member involved, sliall report its findings to the
Council, whose action shall be final.

ARTICLE IV.
Amendments.
Additions to or modifications of this Code may be made accord-
ing to Article VIII of the Constitution.

CONSTITUTION

ARTICLE I,

NAME.

This organization shall be termed,

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

ARTICLE IL

OBJECTS.

The objects of this organization shall be :

To advance the cause of applied chemical science.

To give the profession of Chemical Engineers such standing be-
fore the community as will justify its recognition by Municipal,
State, and j^ationaL authorities in public works.

To raise the professional standard among Chemical Engineers,
discouraging and prohibiting unprofessional conduct.

To cooperate with educational institutions for the improvement of
the education of the men who are to enter this profession.

To encourage original work in chemical technology.

To promote pleasant acquaintance and social and professional
intercourse among its members.

To publish and distribute such papers as shall add to classified
knowledge in chemical engineering and shall increase industrial
activity.

ARTICLE III

MEMBERSHIP

Section 1. {Qualifications for Membership.) Membership
shall consist of two grades: Active and Junior.

Active Membership shall require the following preparation
and training:

All candidates must be not less than 30 years of age and must be
proficient in chemistry and in some branch of engineering as applied
to chemical problems, and must at the time of election be engaged
actively in work involving the application of chemical principles to
the arts. All candidates for admission to this Institute are expected
to have expert Icnowledge of at least one hranch of applied chemistry.
and must fulfill one of the following requirements :

259

260 THE CONSTITUTIOX

1. Candidates who hold no degree from an approved university
or technical school mui-t have had ten years' experience in chemical
technology; five being in responsible charge of operations requiring
the elaboration of raw materials, the design of machinery involving
chemical processes, or the application of chemistry to industry.

2. Candidates who hold the degree of A. B. (Bachelor of Arts)
from an approved university or technical school offering a four-year
course must have had at least eiglit years of practical experience as
outlined under No. 1.

3. Candidates who hold the degree of Ch. E. (Chemical Engi-
neer), B. S. (Bachelor of Science), in Chemistry or Chemical Engi-
neering, or E. E. (Electrical Engineer), C. E. (Civil Engineer), or
M. E. (Mechanical Engineer), or equivalent degrees from an approved
university or technical school offering at least a four-year course,
must have had at least five years' practical experience as outlined
under No. 1.

4. For candidates who in addition hold the degree of Ph. D.
(Doctor of Philosophy) or Sc. D. (Doctor of Science) in Chemistry,
the number of years required to earn the higher degree may be
deducted from the number of years of experience required.

Junior Membership .shall require the following preparation and
training:

All candidates must be not less than 2.3 years of age and must
be engaged, at the time of election, in some branch of applied
chemistry and must fulfill one of the following requirements:

1. Hold the degree of Ch.E. (Chemical Engineer), B.S. (Bachelor
of Science) in Chemistry or Chemical Engineering, E.E. (I'^lectrieal
Engineer), C.E. (Civil Engineer), M.E. (Mechanical Engineer), or
e(]uivalent degree from an approved university or technical school
offering at least a four years' course.

2. Have had five years' experience in Applied Chemistry.

.Junior Members .'^hall have all privileges of the Institute except-
iiin those of voting, holding office, and wearing the emblem or badge
of Active Membership. A .suitable emblem or badge of Junior
Meitibership as adopted by the Institute may be worn by the Junior
i\I(-iiil)( IS. When qualified, a Junior Member may apply for Active
Mcnibership, but must do so before reaching the age of 35, otherwise
his membership shall expire.

Section 2. (Applicationx.) A^\ aiiplications for memlxTship
must be made to the Secretary in writing, and shall embody a concise

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS 261

statement with the dates of the candidate's professional training
and experience, and shall be in a form and in such detail as may
be prescribed by the Membership Committee. The applicant for
Active Membership shall give the names of at least five members to
whom he is personally known. The applicant for Junior Membership
shall give the names of at least five persons to whom he is personally
known, two of whom shall preferably be members of the Institute.
Each of these shall be requested by the Secretary to certify to the
training, experience, professional attainment, and standing of the
api^licant. On receiving a favorable report from at least three of these
references, the applicant shall be eligible to recommendation by the
Membership Committee.

Section 3. {Election of Members.) At stated periods the Sec-
retary shall mail to the members a ballot containing a list of all appli-
cants who have been recommended by the Membership Committee.
This list shall contain a detailed statement of each applicant's career
and the names of the members who have vouched for him. All bal-
lots shall be returned to the Secretary not later than three weeks after
the date of issue. The ballots shall be canvassed by the Meml)ership
Committee, who shall report to the Council, who shall then declare
each applicant elected for whom at least ninety-five per cent, of all
ballots cast are in the affirmative. Provided, however, that anj
member voting in the negative may address a confidential letter to
the Coimcil, stating his objections to the candidate with evidence for
the charges made. If the Council upon investigation considers such
objections valid, they may declare an election void. A rejected candi-
date may make application again any time after one year. Persons
elected to membership shall be notified at once by the Secretary.
They must then subscribe to the rules of the Institute.

Section 4. {Honorary Members.) As the result of unusual
ability and public recognition on the part of the industrial world, a
person may, upon nomination of the Council and a vote of the So-
ciety at large, be made an Honorary Member, but at no time shall
this number exceed five.

Section 5. {Expulsions.) For abuse or misuse of the privileges
of the Institute or conduct unbecoming a member in the opinion of
the Council, a two-thirds vote of the Council may expel any member
of the Institute.

Section 6. {Dues.) The entrance fee for Active Members shall
be $15.00; Junior Members shall pay no entrance fee; Annual dues

262 THE CONSTITUTION

for active members $15.00, for Junior Members $10.00. Junior
Members, on becoming Active Members, shall pay an entrance fee
()' $15.00 less $1.00 per year for each year of their membership as
Junior Members. Provided, however, that no entrance fee shall be
exacted until the membership shall reach 200.

Any member may anticipate his dues for life by paying in ad-
vance such a sum as would be demanded by any reputable insurance
association to yield an annuity equal to the annual dues from the time
of the agreement until death. Upon resignation, or expulsion, all
money so provided is to become the property of the Institute. Any
person joining the Institute after the middle of the fiscal year is re-
quired to pay one-half of the dues only for that year. Any person in
arrears for three months shall be notified by the Secretary. For non-
payment at the e.xpiration of one-half year, a member forfeits the right
to vote or to receive the notices of the Association until dues are paid
in full. All members are considered as such unless actual resignations
are formally presented and accepted with the full payment of dues.
• On account of extenuating circumstances, dues may be remitted to
any member by a two-thirds vote of the Coimcil.
ARTICLE IV.

OFFICERS.

Section 1. The oflficers of this Society shall be a President, three
Vice-Presidcnt.=, a Secretary, a Treasurer, an Auditor, and nine Direc-
tors. The officers shall be elected at the annual meeting. The Presi-
dent shall serve one year, the Vice-Presidents for three years each,
and the Directors for three years each. The Secretary, Treasurer, and
Auditor shall be elected for terms of one year each. At the first an-
nual meeting one Vice-President shall be chosen for one year, one
for two years, and one for three years. Three Directors shall be
chosen for one year, three for two years, and three for three years.
Thereafter, oflficers shall be chosen annually to serve full terms. The
President, Ex-Presidents for the two years succeeding the ex-
piration of their term of office as President, Vice-Presidents,
Secretary, Treasurer, and Directors shall constitute the Council
of the Institute. The President, Vice-Presidents, and Directors
cannot be re-elected within the current twelve months from
the expiration of term. The duties of office begin immediately
after election and notification. An acceptance of office must
be in writing addressed to the Secretan,'. Vacancies occurring
in any office shall be filled by a majority vote of the Council for the

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS 263

unexpired term. The duties of all officers shall l)e such as usually
pertain to their oflfices or may be delegated to them by the Council or
the Institute.

Section 2. (Election of Officers.) After the election at which
this Constitution is adopted, the election of officers shall be by letter
ballot. The Secretary, at least eight (8) weeks prior to each annual
meeting, shall send to every member of the Institute a blank nominat-
ing ballot upon which the member may make nominations for the of-
ficers and Directors to be elected at the coming annual meeting. The
nominating ballot is then to be properly signed and transmitted to
the Secretary not later than five (5) weeks prior to the annual meet-
ing. It shall then become the duty of the Secretary to prepare
and issue an official ballot upon which shall appear the names
of all nominations for office or for Directors which shall have
appeared upon at least ten (10) nominating ballots. Tlie of-
ficial ballots shall be mailed not later than three (3) weeks prior to
the annual meeting, one to each member, who shall properly signify
on it his choice for the various offices and Directors, and transmit it
to the Secretary. At the annual meeting the President shall appoint
tellers to whom the Secretary shall deliver all the ballots received
by him unopened, and who shall count and announce the vote.

ARTICLE V

COUNCIL

The Council shall have supervision and care of all property of
the organization, and shall conduct its affairs according to the Con-
stitution and By-Laws. At each annual meeting it shall present a
statement of its proceedings during the year. Eight members of the
Council called together by notice from the Secretary shall constitute
a quorum, provided, however, that three members may be represented
by proxy.

ARTICLE VI.

ST.VNDING COMMITTEES.

The Council shall appoint the following committees:

1. Finance.

2. Committee on Meetings.

3. Publications.

4. Membership.

5. Library.

6 House Cosimittee.

264 THE COSSTITVTIOX

FINANCE COMMITTEE.

Tlic Finance Committee shall have charge of the financial affairs
of the Institute. This committee must prepare the budget and ap-
prove all expenditures. The Chairman of the Committee may be
the Auditor of the Institute.

MKMRKIiSniP COMMITTEi:.

The Membership Committee shall be constituted of fifteen mem-
bers, ten of whom may vote by proxy at any meeting. To the Mem-
bership Committee all applications for membership shall be referred.
It is the duty of this committee to see that no person is admitted to
the organization who is not qualified.

COMMITTEE ON MEETINGS.

This committee shall have charge of all meetings of the organi-
zation and shall fix dates and places of meeting.

COMMITTEE ON PtTBLICATIONS.

This committee shall look after the papers presented to the In-
stitute. If considered expedient, any or all of these papers may be
published and distributed to members.

LIBKARY COMMITTEE.

This committee shall have charge of all permanent records, books,
papers, pamphlets, etc., and shall obtain and place on file a complete
record of all patent literature in reference to chemical engineering.

HOUSE COMMITTEE.

This committee shall look after the social affairs of the Institute,
fixing the time and place of entertainments.

ARTICLE VII.

MEETINGS.

The annual meeting of the Association shall be held in Decem-
ber, the exact date to be fixed by the Council.

This Institute shall be governed by its Constitution in con-
formity with the laws of the United States. All questions shall be
decided by majority of votes cast. The Institute shall not be held
responsible for opinions expressed in papers. The name or use of
the Institute shall not be tolerated for any commercial purpose.

Upon the adoption of this Constitution officers shall be elected im-
mediately to hold office until the election and installation of their
successors.

AMERICAIS' INSTITUTE OF CHEMICAL ENGINEERS 265

ARTICLE VIII.

AMENDMENTS TO THE CONSTITUTION.

Any member may propose an amendment by addressing the Secre-
tary. At the first regular meeting thereafter the subject shall be dis-
cussed, and if worthy, notice to vote on same shall be posted until the
next regular meeting, and written copy of the notice shall be sent to
each member. The proposed amendment shall then be discussed in
open meeting and can be passed by two-thirds vote of all members of
the Institute as the result of letter ballot.

BY-LAWS

ORDER OF BUSINESS.
Regular Meeting.

Reading of minutes of last stated meeting.

Miscellaneous announcements.

Reading of papers, discussion, and communications.

Adjournment.
Annual Meeting.

Reading of minutes of last stated meeting.

Miscellaneous announcements.

Stated business.

Annual reports.

Election of officers.

Address of retiring President, etc.

Adjournment.

In all questions requiring parliamentary ruling not provided
for by the Rules of the Institute, "Robert's Rules of Order" shall be
the governing authority.

OFFICERS AND COMMITTEES FOR 1913
COUNCIL

Elected at Detroit Meeting, December 7, 191 2
President,

T. B. Wagner New York, X. Y.

Vice-Presidents,

M. C. Whitaker New York. X. Y.

R. K. Meade Baltimore, Md.

G. W. Thompson- Brooklj-n, N. Y.

Secretary,

John- C. Olsen Brooklyn, N. Y.

. Treasurer,

F. W. Frerichs St. Louis, Mo.

A uditor.

Geo. D. Roseng.\rten- Philadelphia, Pa.

Ex-Presidents,

F. \V. Frerichs St. Louis, Mo.

L. H. Baekeland Yonkers, X. Y.

Directors for One Year

Edw. G. Acheson Niagara Falls, N. Y.

\Vm. M. Booth Syracuse, N. Y.

Edw. Hakt Easton, Pa.

Directors for Two Ye.\rs

A. C. Langmuir Brookl\ii, N^. Y.

H. S. Miner Gloucester City, X. J.

A. Bement Chicago, 111.

Directors for Three Yeaks

Geo. D. Rosengarten Philadelphia, Pa.

JOKICHI Takamine Xew York, X. Y.

Jas. R. Withrow Columbus. Ohio

266

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS 267

COMMITTEE ON PUBLICATIONS

Frerichs, F. W., Chairman Kippenberg, Henrs

Andrews, Launcelot W. Olsen, J. C.

Hart, Edward Ittner, M. H.

Bain, J. Watson

MEMBERSHIP COMMITTEE

Langmuir, a. C, Chairman Rosengarten, Geo. D.

Adamson, Geo. P. Kaufmann, H. M.

Bassett, Wm. H. Miner, H. S.

Converse, W. A. Olney, L. A.

DeCew, J. A. Richards, J. W.

Dow, a. W. Robertson, A.

Ittner, M. H. " Thompson, G. W.

CHAIRMEN OF LOCAL COMMITTEES ON MEMBERSHIP

Frerichs, F. W St. Louis, Mo.

Belden, a. W Pittsburgh, Pa.

LiHME, LP Cleveland, Ohio

Rosengarten, Geo. D Philadelphia, Pa.

Byers, H. G Seattle, Wash.

Parker, T. J New York, N. Y.

Little, A. D Boston, Mass.

Converse, W. A ' Chicago, 111.

COMMITTEE ON CHEMICAL ENGINEERING EDUCATION

WiTHROw, Jas. R., Chairman Whitaker, M. C.

Booth, Wm. M. Wiechmann, F. G.

Sadtler, Samuel P.

COMMITTEE ON MEETINGS

Sadtler, Samuel P., Chairman Langmuir, A. C.

Booth, Wm. M. Meade, R. K.

Minor, John C, Jr. Olsen, J. C.

Howard, Henry Sadtler, S. S.

268 AMERICA!^ INSTITUTE OF CHEMICAL ENGINEERS

COMMITTEE ON BOSTON MEETING

Howard, Henry, Chairman Olney, L. A.

Chas. a. Catlin Sharples, S. P.

Little, A. D. Tuorp, F. H., Secretary

FINANCE COMMITTEE

Thompson, G. W., Chairman McKenna, Chas. F.

TocH, Maximilian Elliott, A. H.

COMMITTEE ON MEDAL

Booth, Wm. M., Chairman Robertson, A.

Richards, J. W. Sadtler, Samuel P.

COMMITTEE ON STANDARDIZATION OF BOILER TESTS

Bement, A. Campbell, J. H.

Booth, Wm. M. Prentiss, George N.

LIBRARY COMMITTEE

Alexander, Jerome, Chairman Myers, Ralph E.

Olsen, J. C.

COMMITTEE ON PATENTS

Baekeland, L. IL, Chairman Toch, Maximilian

Grosvenor, Wm. M. Whitaker, M. C.

COMMITTEE ON PUBLIC POLICY

McKenna, Chas. F., Chairman Taylor. Edw. R.

Frerichs, F. W. Parker, Thos. J.

Baekeland, L. II. Takamine, Jokichi

COMMITTEE ON ETHICS

Thompson, G. W., Chairman, 5 yrs. Little, A. D., 2 yrs.

4 yrs. Langmltr, A. C, i yr.

McKenna, Chas. F., 3 yrs.

LIST OF MEMBERS: JUNE, 1913

Honorary Member
Chandler, Chas. F., Columbia University, New York City.

Active Members
ACHESON, Edward G., Niagara Falls, N. Y.

President, International Acheson Graphite Co.
Adamson, George P., 233 Reeder St., Easton, Pa.

Vice-President and General Manager, The Baker and Adamson Chem-
ical Co.
Adgate, Matthew, Naugatuck, Conn.

Supt. of the Naugatuck Chemical Co.
Alexander, D. B. W., iooo Date St., Los Angeles, Cal.

Pacific Coast Chemist for The Barber Asphalt Paving Co.
Alexander, Jerome, 502 West 45th St., New York City.

Treasurer and Chemist, National Gum and Mica Co., National Glue
and Gelatin Works.
Allen, Lucius E., Box 22, Belleville, Ont., Can.

Consulting Chemical Engineer, Managing Director Ontario Limestone
and Clay Co., Ltd., BelleviUe, Ont.
Anderson, Louis J., 315 Burke St., Easton, Pa.

Chemical Engineer, Alpha Portland Cement Co., Easton, Pa.
Andrews, Launcelot W., Davenport, la.

President, Andrews Chemical Works.
Arnold, Charles E., 602 West 20th St., Wilmington, Del.
Austin, Herbert, 485 North Main St., Fall River, Mass.

Chemical Engineer and Partner Manager of Ernest Scott & Co., of
Fall River, Mass., and Montreal, P. 0.
Ayer, Arthur W., 3403 Gray's Ferry Rd., Philadelphia, Pa.

General Supt., Harrison Bros. & Co.
Baekeland, Leo H., Yonkers, N. Y.

Research Chemist and Chemical Engineer.
Bain, J. Watson, Uni\-ersity of Toronto, Toronto, Can.

Associate Professor of Applied Chemistry.
Baied, Wm. H., 1199 Woodward Ave., Detroit, Mich.

Secretary, Larrowe Construction Co.
269

270 AMERICAN IXSTITUTE OF CHEMICAL ENGINEERS

Baker, John T., Phillipsburg, N. J.

President, J. T. Baker Chemical Co.
Barton, G. E., 227 Pine St., Millville, N. J.

In charge of Laboratory and Dept. Mfg. Glass, Whitall Tatum Co.
Baruch, Edgar, 806 Wright & Callender Bldg., Los Angeles, Cal.

Consulting Chemical Engineer.
Bartow, Edward, Urbana, 111.

Professor of Analytical Chemistry, Univ. of 111. Director of State
Water Survey of Illinois. Consulting Chemist with the Davenport
Water Co.
Bassett, William H., Cheshire, Conn.

Metallurgist, American Brass Co.
Bebie, J., 1800 South 2d St., St. Louis, Mo.

Chemical Engineer, Monsanto Chemical Works.
Beck, Arthur G., care Canada Cement Co.

Exchaw, Alberta, Canada.
Becnel, Le7IN A., 51 Arabella St., New Orleans, La., P. O. Box 390.

Chemical Engineer and Consulting Chemist.
Beers, Frank T., Washburn, Wis.

Supt. Barksdale Plant, E. I. du Pont de Nemours Powder Co.
Behrend, Otto F., Erie, Pa.

Vice-President and Treasurer, Hammermill Paper Co.
Belden, a. W., Bureau of Mines, 40th & Butler Sts., Pittsburgh, Pa.

Engineer in Charge.
Bement, a., 206 S. LaSalle St., Chicago, 111.

Consulting Mining and Mechanical Engineer.
Booth, L. M., 136 Liberty St., N. Y.

President and Director, L. M. Booth Co., New York.
Booth, William M., Dillaye Building, Syracuse, N. Y.

299 Broadway, Xcw York, Consulting Chemist and Engineer.
Bower, Willlam H., 2815 Gray's Ferry Rd., Philadelphia, Pa.

First Vice-President of Henry Bower Chemical Mfg. Co.
Brooks, Percival C, General Chemical Co., Chicago Heights, 111.

Asst. Supt., Illinois Works, General Chemical Co., Chicago Heights,
Illinois.
Brown, H. F., Room 915, du Pont Bldg., Wilmington, Del.

Chemical Director, Smokeless Powder Dept., E. I. du Pont de Ne-
mours Powder Co.
Bragg, E. B., Evanston, 111.

Vice-President and Manager of General Chemical Co., Chicago
Branch.
Byers, Horace G., Seattle, Wash.

Professor Chemistry, University of Washington, Consulting Chemical
Engineer.

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS 271

Camp, J. M., Chief Bvtreau of Instruction, Carnegie Steel Co., Carnegie

Steel Co., Carnegie Bldg., Pittsburgh, Pa.
Campbell, John Hayes, i6i N. Catherine Ave., La Grange, 111.

Chemical and Metallurgical Engineer, 2200 Insurance Ex., Chicago,
111.
Catlln, Charles A., 133 Hope St., Providence, R. I.

Chief Chemist and a Director of the Rumford Chemical Works.
Chute, Harry O., 197 Pearl St., New York. Chemical Engineer.

Converse, William A., 2005 McCormick Building, Chicago. 111.

Chemical Director Dearborn Drug & Chemical Works.
Conner, Arthur B., 217 W. Boulevard, Detroit, Mich.

Chief Chemist and Chemical Engineer for Detroit Chemical Works,
Detroit, Mich.
Corse, Wm. M., Sycamore St., & N. Y. C. Belt Line, Buffalo, N. Y.

Works Manager, Lumen Bearing Co., Buffalo, N. Y.
Crowley, Chas. P., Omaha, Neb.

Gas Commissioner of the City of Omaha, Neb.; Professor of Chem-
istry, Creighton Medical College.
Cushman, Allerton S., 19th and B Sts., N. W., Washington, D. C.

Director and President, Institute of Industrial Research.
Dailey, J. G., c, o CHnchfield Fuel Co., Spartanburg, S. C.

Chemical Engineer, CUnchfield Fuel Co., Spartanburg, S. C.
Dannenbaum, Herman, Frankford, Philadelphia, Pa.

Vice-President National Ammonia Co.
Davoll, David L., Jr., 765 Westminster Road, Brooklyn, N. Y.

Chief Chemist, Henry Heide, 313 Hudson St., New York, N. Y.
Dean, John G., Box 610, Los Angeles, Cal.
DeCew, J. A., Canadian Express Bldg., Montreal, Canada.

Consulting Chemical Engineer.
Diller, H. E., c/o General Electric Co., Erie, Pa.

Chemist and Metallurgist, Research Laboratory, General Electric
Co., Erie, Pa.
Dow, A. W., 131 E. 23d St., New York, N. Y.

Member of the firm of Dow & Smith, Consulting Engineers.
Elliott, A. H., 52 E. 41st St., New York, N. Y.

Consulting Engineer.
Ellis, Carleton, 92 Greenwood Ave., Montclair, N. J.

Consulting Chemist and Inventor.
Foersterling, Hans, 380 High St., Perth Amboy, N. J.

Second Vice-President, Roessler & Hasslacher Chemical Co.
Fowler, Theodore V., Box 15, Buffalo, N. Y.

Supt. of the Buffalo Works of the General Chemical Co.
Frasch, Herman, 17 Battery Place, New York, N. Y.

President Union Sulphur Co., 17 Battery Place, New York, N. Y.

272 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

French, Edw. H., Smethport, Pa.

Chemical Engineer, Hilton & French, Smethport Research and
Testing Laboratories.
Frerichs, F. W., 4320 Washington Bou., St. Louis, Mo.

Vice-President, Herf & Frerichs Chemical Co.
GiBBS, A. E., c/o Permsylvania Salt Mfg. Co., Greenwich Point, Phila., Pa.
Glover, H. Lester, 73 W. Johnson St., Germantown, Phila., Pa.

Supt. of the Falls of Schuylkill Works of the Powers-Weightman-
Rosengarten Co.
Gray, Chas. W., Driftwood, Pa.

Consulting Chemist, Keystone National Powder Co.
Greth, J. C. Wm., Pittsburgh, Pa.

Manager, Water Purifying Dept. of William B. Scaife & Sons Co.
Griswold, Thomas, Jr., Midland, Mich.

Engineer, The Dow Chemical Co.
Secretary, The Midland Chemical Co.
Grosvenor, Wm. IVL, 50 E. 41st St., New York City.

Consulting Chemist and Factory Engineer.
GtTDEMAN, Edward, 903-4 Postal Telegraph Bid., Chicago, 111.

Consulting Chemist and Chemical Engineer.
Haanel, Eugene, Dept. of Mines, Ottawa, Ont., Can.

Director of Mines, Dept. of Mines, Ottawa, Ont., Can.
Harriman", Norman F., Union Pacific Laboratory, Omaha, Neb.

Chemist and Engineer of Tests, Union Pacific R. R. Co.
Hart, Edward, Easton, Pa.

Prof. Chemistry, Lafayette College; President Baker & Adamson
Co.; Prop. Chem. Pub. Co.; Consulting Engineer.
Hebden, John C, Bo.x 465, Providence, R. L

Vice-President and General Manager, Franklin Process Co.
Herreshoff, J. B. Francis, 620 West End Ave., New York, N. Y.

Vice-President Nichols Copper Co., Consulting Engineer General
Chemical Co.
Holland, Wm. R., Gloucester City, N. J.

Foreman of the Chemical Dept., Welsbach Light Co., and Assistant
to Chief Chcmi.st.
Hollander, Charles S., Hartford, Conn.

Secretary and Chief Chemist, Eastern Chemical Works, Inc., Hart-
ford, Conn.
HoSKiNS, Wm., Ill W. Monroe St., Chicago, 111.

Mariner & Hoskins, Consulting Chemical Engineers.
Howard, Henry, ^^ Broad St., Boston, Mass.

Vice-President, Merrimac Chemical Co.
Hughes, L. S., 1246 Dearborn Ave., Chicago, 111.

Chemist Illinois Steel Co.

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS 273

Humphrey, H. C, 17 Battery PI., New York City.

Chief Chemist, Eastern Branch, Com Products Refining Co.
Ittner, Martin H., Colgate & Co., Jersey City, N. J.

Chief Chemist, Colgate & Co.
James, Joseph H., Pittsburgh, Pa.

Prof. Chemical Engineering Practice, Carnegie Technical Schools.
Jones, A. B., 981 Central Ave., Plainfield, N. J.

Supt. Laurel Hill and Bayonne Works, General Chemical Co.
Jones, L. C, Syracuse, N. Y.

Laboratory Manager, Solvay Process Co., and Semet Solvay Co.;
Vice-President, Solvay CoUeries Co.
Kaufmann, H. M., 55 John St., New York, N. Y.

General Manager, Mutual Chemical Co. of America.
Kilmer, Frederick Barnett, 147 College Ave., New Brunswick, N. J.

Director of Laboratories, Johnson & Johnson, New Brunswick,
N.J.
KiMMEL, H. R., 517-519 Superior Bldgs., Cleveland, Ohio.

Consulting Chemical Engineer, Industrial Testing Laboratory.
Kingsbury, Percy C, 50 Church St., New York, N. Y.

Chief Engineer German-American Stoneware Works, 50 Church St.,
New York City.
Kippenberg, Henry, 15 Darmstadt Ave., Rahway, N. J.

Supt. of Chemical Manufacture at Rahway Plant of Merck & Co.
Kremer, Waldemar R., Vilter Mfg. Co., Milwaukee, Wis.

Electrical-Mechanical Engineer.
Lamar, William Robinson, 8-14 Johnson St., Newark, N. J.

President, Lamar Chemical Works.
Langmuir, Arthur C, 9 Van Brunt St., Brooklyn, N. Y.

Supt. Factory, Manx & Rawolle.
Larkin, E. H., 3600 N. Broadway, St. Louis, Mo.

Director, National Ammonia Co., St. Louis, Mo.
Lazell, E. W., 426 Railway Exchange Bldg., Portland, Ore.

Edwards & Lazell, Consulting and Chemical Engineers.
Lee, Fitzhugh, Gr.asseUi Chemical Co., Cleveland, Ohio.

Assistant Chairman Manufacturing Committee, Grasselli Chemical Co.
Le Maistee, F. J., Ridley Park, Del. Co., Pa.

Chemical Engineer, E. L du Pont de Nemours Powder Co.
Lessner, C. B., Carril, Spain.

Manager of the Carril Works and Chemist to the San Finx Tin Mines,
Ltd., and Metallurgical Chemist to the AngeUta Mines.
Le Sueur, Ernest A., 50 McLaren St., Ottawa, Ont., Can.

General Manager and President of the General Explosives Co., Ltd.
LiHME, Tens P., Grasselli Chemical Co., Cleveland, Ohio.

Engineer, Grasselli Chemical Co,

274 AMERICAN ISSTITUTE OF CHEMICAL ESCI SEERS

LiNDER, Oscar, 56 North Waller Ave., Chicago, 111.

Works Chemist, Western Electric Co., Hawthorne Works.
Little, A. D., 93 Broad St., Boston, Mass.

President and General Manager, Arthur D. Little, Inc., Chemists and

Engineers.

President and General Manager, Chemical Products Co., Boston,

Mass.
LuNDTEiGEN, A., c/o Ash Grove Lime & Portland Cement Co., Kansas

City, Mo.

Managing Engineer, Ash Grove Lime & Portland Cement Co.,

Kansas City, Mo.
Mallinxkrodt, Edward, St. Louis, Mo.

President Mallinckrodt Chemical Works.
Marsh, Clarenxe W., Niagara Falls, N. Y.

Chief Engineer The Development and Funding Co., New York City.
Mason, William P., Troy, N. Y.

Prof. Chemistry, Rensselaer Polytechnic Institute.
Matos, Louis J., 103 No. 19th St., E. Orange. N. J.

Technical Chemist and Chemical Engineer with the Cassella Color

Co., 182 Front St., New York City.
MacNaughton, Wm. G., Port Edwards, Wis.

Assistant to General Manager in charge of manufacturing, Nekoosa

Edwards Paper Co.
McCormack, Harry, Armour Institute, Chicago, 111.

Professor of Chemical Engineering, Armour Institute of Technology,

Chicago, 111.; Editor of the Chemical Engineer; Consulting Chemist

and Chemical Engineer.
McKenna, Chas. F., so Church St., New York. N. Y.

Consulting Chemist and Chemical Engineer.
AIeade, Richard K., Roland Park, Baltimore Co., Md.

Consulting Chemical Engineer.
Metz, Gustave p., 95 Elm St., Montclair, N. J.

Supt. and Vice-President, Consolidated Color and Chemical Co.,

Newark, N. J.
■Miller, A. L., 1104 Foulkrod St., Frankford, Philadelphia, Pa.

Supt. Chem. Dept., Barrett Mfg. Co.
Mills, Jas. W., 2201 C St., Granite City, 111.

Asst. Supt. Open Hearth Department Granite City Steel Works

Branch of the National Enameling and Stamping Co.
Mixer, H. S., Gloucester City, N. J.

Chief Chemist Welsbach Light Co.
Minor, Johx C, Jr., 50 Church St., New York, N. Y.

Manager, General Carbonic Acid Co.
Myers, Ralph E., 31 Franklin Ave., East Orange, N. J.

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS 275

Newhall, Chas. a., 603 Northern Bank Bldg., Seattle, Wash.

Senior Member of Newhall, Smith & Co., Chemical and Efficiency
Engineers, Geologists.
Olney, Louis A., Lowell Textile School, Lowell, Mass.

Professor of Chemistry and Head of the Department of Textile
Chemistry and Dyeing, Lowell Textile School; President Stirling
Mills, Lowell, Mass.
Olsen, John C, Polytechnic Institute, Brooklyn, N. Y.

Prof, of Analytical Chemistry; Consulting Chemist.
Parker, Thomas J., 25 Broad St., New York City.

Chemical Expert of the Sales Department of the General Chemical Co.
-Peckham, Stephen F., 150 Halsey St., Brooklyn, N. Y.
Porter, J. Edward, Box 785, Syracuse, N. Y. Chemical Engineer.

Prentiss, George N., 226 33d St., Milwaukee, Wis.

Chief Chemist, C, M. & St. P. R. R.
Puckhaber, Geo. C, 805 Prospect Place, Brooklyn, N. Y.

Glue Maker and General Manager of Glue Department, Moller &
Co., Maspeth, N. Y.
Richards, J. W., University Park, South Bethlehem, Pa.

Professor of Metallurgy, Lehigh University; Secretary American
Electrochemical Society; President Electrochemical Publishing Co.
Reese, Charles Lee, 725 du Pont Building, Wilmington, Del.

Chemical Director, High Explosives Operating Dept., E. L du Pont de
Nemours Powder Co.
Robertson, Andrew, 2 N. gth St., Richmond, Va.

Member of firm Froehling & Robertson, Consulting Chemists and
Chemical Engineers.
Roessler, Franz, 89 High St., Perth Amboy, N. J.

Vice-President and Secretary, Roessler & Hasslacher Chemical Co.
Rosengarten, Geo. D., Box 1625; Philadelphia, Pa.

Vice-President The Powers-Weightman-Rosengarten Co.
Prochazka, George A., 138 West 13th St., New York.

General Manager Central DyestufT Chemical Co., Newark, N. J.
Sadtler, Samuel P., 39 South loth St., Philadelphia, Pa.

Prof. Chemistry, Philadelphia College of Pharmacy, and Consulting
Chemist (Samuel P. Sadtler & Son).
Sadtler, Samuel S., 39 South loth St., Philadelphia, Pa.

Samuel P. Sadtler & Son.
Schanche, H. G., 3500 Gray's Ferry Road, Philadelphia, Pa.

Chemical Director, Harrison Bros. & Co. Inc., Philadelphia, Pa.
SCHROEDER, C. M. Edw., Rutherford, N. J.

Consulting Chemist, 34 Bloomfield Ave., Passaic, N. J.
Sharples, Stephen P., 26 Broad St., Boston, Mass.

Analytical and Consulting Chemical Engineer and Assayer.

27G AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

Shattuck, a. Forrest, Detroit, Mich.

Chief Chemist, Solvay Process Co.
SiiiMER, Porter W., Easton, Pa.

Proprietor and Chief Chemist of Chemical Laboratory.
Simmons, W. H., Fenton, Mich.

Superintendent, New Aetna Portland Cement Co.
Simpson, Edward H., Westside Ave, Jersey City, N. J.

Manager, Arlington plant of the Mutual Chemical Co. of America.
Smith, Albert W., 7901 Euclid Ave., Cleveland, O.

Professor of Chemistry and Director of the Chemical Laboratory
of Case School of Applied Science.
Smith, Francis Pitt, 131-133 East 23d St., New York, N. Y.

Member of the firm of Dow & Smith, Chemical Engineers.
Smith, Harry E., 36 Beeresford PL, East Cleveland, Ohio.

Chemist and Engineer of Tests, Lake Shore & Michigan Southern Ry.
Smith, Theodore E., 54 Hudson Place, Weehawken, N. J.

Supt. Oil Dept., Com Products Refining Co., Edgewater, N. J.
Smith, Thorn, 125 Langley Ave., Detroit, Mich.

Diack & Smith, Consulting Chemists.
Stillman, John Maxson, Stanford Univ., Cal.

Professor of Chemistry.
Takamine, Jokichi, 520 West 173d St., New York City.

Consulting Chemist for Parke-Davis & Co., Detroit, Mich.
Taylor, Edward R., Penn Yan, N. Y. Manufacturing Chemist.

Taylor, John, 137 S. New St., Bethlehem, Pa.
Teas, William H., Ridgway, Pa.

General Supt., U. S. Leather and Allied Companies.
Thompson, Gustave W., 129 York St., Brooklyn, N. Y.

Chief Chemist, National Lead Co.
Thomson, Henry N., Tooele, Utah.

Superintendent and Consulting Metallurgical Engineer, Tooele
Plant, International Smelting & Refining Co.
Thorp, Frank H., Boston, Mass.

Asst. Prof. Industrial Chemistrj% Mass. Inst. Tech.
Thiele, Ludwig a., Holland, Mich.

General Manager of the Holland Gelatine Works, Holland, Mich.
Toch, Maximilian, 320 Fifth Ave., New York City.

Member of firm of Toch Bros.
Trautwein, a. p., Carbondale, Pa. Pres. Carbondalc Instrument Co.

Tufts, John L., Winchester, Mass. Chemical Engineer.

Tyson, George N., 2S15 Gray's Ferry Rd., Philadelphia, Pa.

Supt. for the Henry Bower Chemical Manufacturing Co.
Veillon, a. a. L., 1800 South 2d St., St. Louis, Mo.

Vice-President and Works Manager, Monsanto Chemical Works.

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS 277

VoRCE, L. D., 364 W. Grand Boulevard, Detroit, Mich.

Supt. of Pennsylvania Salt Mfg. Co., Supt. of Goldschmidt Detirming
Co., Gen. Supt. Wyandotte Southern Ry. Co.
Wagner, Theodore B., 17 Battery Place, New York, N. Y.

Operating Committee, Com Products Refining Co.
Warren, Robt. C, 214 E. 5th St., Little Rock, Ark.

Chemical Engineer for the Arkansas Cotton Oil Co.
Watson, John R., P. O. Box 6, LaPlata, Md.
Wesson, David, m South Mountain Ave., Montclair, N. J.

Manager Tech. Dept. Southern Cotton Oil Co., 24 Broad St., New York.
Wheeler, Frank G., 778 FrankUn St., Appleton, Wis.

Chemist with the Penn. Salt Mfg. Co., Wyandotte, Mich.
Whitaker, M. C, Columbia Univ., New York City.

Professor of Engineering Chemistry, Columbia Univ. Editor of
Jour, of Ind. and Eng. Chemistry, Consulting Chemical Engineer.
White, Fred. S., 392 Clinton Ave., Brooklyn, N. Y.

Supt. Glycerine Dept., Marx & Rawolle, Brooklyn, N. Y.
Wiechmann, Ferdinand G., 39 W. 38th St., New York, N. Y.

Consulting Chemical Engineer.
Williams, Frank M., 43-44 Sherman Bldg., Watertown, N. Y.

Consulting Chemical Engineer and Industrial Chemist.
WiTHROW, Jas. R., Columbus, O.

Professor of Chemistry, Oliio State University, Columbus, 0.
Wood, F. J., 361 Henry St., Brooklyn, N. Y.

Chief Engineer, Marx & Rawolle.
WuRSTER, 0. H., Toronto, Canada.

Assistant Works Manager, Lever Bros., Ltd., Toronto.
Zinsser, Frederick G., Hastings-on-Hudson, N. Y.

Manufacturing Chemist under firm of Zinsser & Co.
ZiTKOwsKi, Herman E., Rocky Ford, Colo.

Chief Chemist and Technical Adviser, American Beet Sugar Co.,
Denver, Colo.
ZwiNGENBERGER, O. K., P. O. Box 112, Perth Amboy, N. J.

Patent Dept., Roessler & Hasslacher Chem. Co.

278 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS

JUNIORS

Allen, William P., 83 Aberdeen Place, Woodbury, N. J.

Chemist, E. I. du Pont de Nemours Powder Co.
BiCKNELL, R. S., SO E. 41st St., New York, N. Y.

Chemical Engineer, The Thermal Syndicate, Ltd., New York City, N. Y.
BovLSTON, Arthur C, 3600 N. 2d St., St. Louis, Mo.

Chemist in charge of ALanufacturing with the Mallinckrodt Chemical

Works.
BuCKMAN, Henry H., Indianapolis, Ind.

Chief Chemist, American Hominy Co.
Caaipbell, Charles L., Wallaston, Norfolk Co., Mass.

Chemical Engineer, with E. B. Badger & Sons Co., 75 Pitts St.,

Boston, Mass.
Clark, Wm., Crafton, Pa.

Metallurgist and Chief Chemist, American \'anadium Co.
Fales, H. a., 308 Schermerhorn St., Brooklyn, N. Y.

\'ice-President and Secretary of The W. H. Fales Co.
■Gage, R. M., The Oaks, Springfield, Mass.

Chemical Engineer, The Fisk Rubber Co., Chicopee Falls, Mass.
GuiLLAUDEU, Arthur, Cincinnati, O.

Chemist and Asst. Supt., The M. Werk Co., 408-432 Poplar St.,

Cincinnati, O.
Heinrich, E. 0., 3214 North 30th St., Tacoma, Wash.

Consulting and Manufacturing Chemist; Director of the Heinrich

Technical Laboratories.
Jordan, Harry E., 113 Monument Place, Indianapolis, Ind.

Sanitary Engineer, Indianapolis Water Co.
Lane, Fred. H., HoUis, L. I., N. Y.

Chemical Superintendent, Emil Caiman & Co., \'emon and Harrison

Aves., Long Island City, N. Y.
Lawrence, Jas. C, P. O. Box 812, Memphis, Tenn.

Consulting Chemical Engineer, Directing Engineer, Forest Product.

Chemical Co., Memphis, Tenn.
Lunn, Charles Albert, Brunswick, Ga.

Chemical Engineer, The Yaryan Naval Stores Co.. Brunswick, Gas
Lunt, G. p., 7S Pitts St., Boston, Mass.

Chemical Engineer, E. B. Badger & Sons Co.
McIntyre, a. G., 404 McGill Bldg., Montreal, Canada.

Chief, Forest Products Laboratories of Canada. Editor, Pulp and

Paper Magazine of Canada.
Meade, George P., Gramercy, La.

Asst. Supt. and Chief Chemist, Gramercy Refinery, Colonial Sugar Co.

AMERICAN INSTITUTE OF CHEMICAL ENGINEERS 279

MiTKE, Charles A., Box 1226, Dawson, N. M.
Peterson, Charles Albert, Lancaster, Pa.

Chief Chemist in the linoleum dept. of the Armstrong Cork Co.,

Lancaster, Pa.
Plumb, Roy A., 58 Lafayette Ave., Detroit, Mich.

Director of Michigan Technical Laboratory, 5S Lafayette Boul.,

Detroit, Mich. .
ScHAEFFER, John A., Joplin, Mo.

Chief Chemist, Picher Lead Co., Joplin, Mo.
Seaman, E. H., Wantagh, L. L

Insurance Engineer, with Underwriters at American Lloyds.
Shreve, R. Norris, care Lamar Chemical Works, Newark, N. J.
Summers, Frank P., 1525 Winnemac Ave., Chicago, 111.

Chemist in charge, Abbott Alkaloidal Co., Chicago, 111.
Turner, Norman L., Belleville, Ontario, Can.

Provincial Assayer of Ontario, Can.
Van Doren, Willard V., 1646 Garfield Boulevard, Chicago, 111.

Superintending Chemist of the plant of the Illinois Vinegar Mfg.

Co., 4Sth St. & Oakley Ave., Chicago, 111.
Whitcomb, L. R., 100 William St., New York.

Chemist and Bacteriologist in charge of Testing Lab., for Nicholas

S. Hill, Jr.

INDEX

PAGE

Acetylene, solubility of 137

solvents for 133

Acetaldehyde as solvent for acetylene 140, 143, 144, 145

Acetone as solvent for acetylene 141

Action of disinfectants on sugar solutions 88

Asphaltic rocks of the United States and their use in street paving 245

Asphalts and petroleums, the presence of oxygen in 178

Availability of blast-furnace slag as a material for building brick 204

Baekeland, L. H., Phenol-Formaldehyde Condensation Products i

Protection of Intellectual Property in Relation to Chemical Industry 19

Bagasse 229

Bakelite i

Beehive coke oven industry of the United States 78

Beet sugar, process of manufacture 222

Belden, A. W., the beehive coke oven industry of the Unted States 78

Blast-furnace slag, availability of as a material for building brick 204

Booth, Wm. M., the chemical engineer and industrial efficiency 184

water for industrial purposes 197

Building brick. Availability of blast-furnace slag as a material for 204

tests for ■ 208

Campbell, John Hayes, The need of standard specifications in oils for

paving block impregnation 170

Cane sugar, process of manufacture of 225

Chemical control and technical accounting in sugar manufacture 220

Chemical engineer and industrial efficiency 184

Chemical engineering course and laboratories at Columbia University. 150

Chemical investigation of Asiatic rice 70

Code of Ethics 255

Coggeshall, Geo. W., and A. S. Cushman, Production of available potash

from the natural silicates 52

281

282 INDEX

PACK

Columbia University, New chemical engineering course and laboratories

at ISO

Column still and extractor i $8

Committees for 1913 267

Constitution 250

Control of initial setting time of Portland cement 119

Creosote oil, Analyses of 1 74

Cushman, A. S., Study of the temperature gradients of setting Portland

cement 43

and Geo. W. Coggeshall, production of available potash from the natu-
ral silicates 52

and H. C. Fuller, Chemical investigation of Asiatic rice 70

Davoll, Jr., David S., Technical accounting and chemical control in sugar

manufacture 220

Decomposition of linseed oil during drying 100

Disinfectants, action of, on sugar solutions 88

Drinking water 2co

Effect of "lime sulphur" spray manufacture on the eyesight 127

Ester-ketone-aldehyde as solvent for acetylene 142

Ethics, Code of 255

Feldspar, potash, silica, and alumina from 68

Formaldehyde, action of phenol on 8

Fuller, H. C, and A. S. Cushman, a chemical investigation of Asiatic

rice 70

Hart, Edward, potash, silica, and alumina from feldspar 68

Industrial efficiency and the chemical engineer 184

Industrial purposes, water for 197

Intellectual property, protection of in relation to chemical industry. ... 19

James, J. H., acetylene solvents i33

" Lime sulphur " spray manufacture, effect of on the eyesight 127

Linseed oil, decomposition of, during drying 100

Manufacture, statistics of 192

Massecuite 23S

Meade, Geo. P., Action of disinfectants on sugar solutions 88

Members for 1913 269

INDEX 283

PAGE

Notes on a study of the temperature gradients of setting Portland cement . 43

Officers for 1913 266

Olsen, J. C, and A. E. Ratner, decomposition of linseed oil during dry-
ing 100

Opacimeter, Thompson's iii

Opacity and hiding power of pigments, tests on 108

Oxygen in petroleums and asphalts 178

Paper laboratory 160

Patent, question, discussion of 37

sysU-m of the United States 21

Paving block impregnation, need of standard specifications for oils in . . . 170
Peckham, S. F., the asphaitic rocks of the United States and their use

in street paving 245

Petroleums and asphalts, the presence of oxygen in 178

Phenol-Formaldehyde condensation products i

Pigments, tests on the opacity and hiding power of 108

Portland cement, control of initial setting time of 119

Notes on a study of the temperature gradients of the setting of 43

Potash, from natural silicates, processes proposed for 57

production of, from the natural silicates 52

silica and alumina from feldspar 68

Production of available potash from the natural silicates 52

Protection of intellectual property in relation to chemical industry 19

Ratner, A. E., and J. C. Olsen, decomposition of hnseed oil during drying 100

Rice, Chemical investigation of 70

Composition of 72, 76

Sadtler, Sam. P., The presence of oxygen in petroleums and asphalts. . . 178

Shelf drier and vacuum pumps 159

Silicates, production of potash from 52

Standard specifications in oils for paving block impregnation 170

Sugar, analysis of raw material for 228

manufacture, technical accounting and chemical control in 220

solutions, action of disinfectants on 88

table of purities for 244

Table of Purities for sugar 244

Technical accounting and chemical control in sugar manufacture 220

Temperature gradients of setting Portland cement 43

Tests on the opacity and hiding power of pigments 108

284 INDEX

PACB

Thompson, G. W., Tests on the opacity and hiding power of pigments. io8

Thompson's opacimcter iii

Vacuum pans iS7

Ware, E. E., control of initial setting time of Portland cement 119

Water for industrial purposes 197

Whitaker, M. C, New chemical engineering course and laboratories at

rolumbia University 150

White, Albert E., Availability of blast-furnace slag as a material for

building brick 204

Withrow, James R., The effect of "lime sulphur" spray manufacture on

the eyesight 127

TP

1

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